英语翻译Experimental SectionSynthesis of 7/8-Hydroxycarbonylalloxazine (5).To a stirredsolution of 3,4-diaminobenzoic acid (3,3.04 g,20 mmol) in 170mL of acetic acid were added boric acid (1.36 g,22 mmol) andalloxane (4) monohydrate (3.36 g,21 mm

英语翻译Experimental SectionSynthesis of 7/8-Hydroxycarbonylalloxazine (5).To a stirredsolution of 3,4-diaminobenzoic acid (3,3.04 g,20 mmol) in 170mL of acetic acid were added boric acid (1.36 g,22 mmol) andalloxane (4) monohydrate (3.36 g,21 mm
英语翻译
Experimental Section
Synthesis of 7/8-Hydroxycarbonylalloxazine (5).To a stirred
solution of 3,4-diaminobenzoic acid (3,3.04 g,20 mmol) in 170
mL of acetic acid were added boric acid (1.36 g,22 mmol) and
alloxane (4) monohydrate (3.36 g,21 mmol).The reaction was
stirred for 3 h at room temperature after which the precipitated
product was filtered off and washed,first with acetic acid then with
diethyl ether,water,and last diethyl ether.The product 5 (green
powder) was isolated in a 3:2 ratio of the 7- and 8-isomer in
quantitative yield.Major isomer:1H NMR (400 MHz,DMSOd6)
ä 12.02 (s,1H),11.79 (s,1H),8.29 (d,J ) 1.9 Hz,1H),8.18
(d,J ) 8.8 Hz,1H),8.09 (dd,J ) 1.9,8.8 Hz,1H).Minor isomer:
1H NMR (400 MHz,DMSO-d6) ä 12.06 (s,1H),11.80 (s,1H),
8.55 (d,J ) 2.0 Hz),8.25 (dd,J ) 2.0,8.8 Hz,1H),7.90 (d,J )
8.8 Hz,1H).13C NMR (DMSO-d6,100 MHz) for the mixture ä
167.0,167.0,160.8,160.8,150.7,150.7,148.6,148.1,145.4,142.5,
141.4,138.8,135.1,134.0,133.7,132.8,132.5,131.1,130.8,129.1,
128.0,127.9.
Synthesis of N1,N3-Dimethyl-7/8-methoxycarbonylalloxazine
(6).9 To a stirred solution of 7/8-hydroxycarbonylalloxazine (5)
(2.58 g,10 mmol) in 500 mL of dimethylformamide (DMF) were
added potassium carbonate (K2CO3) (4.70 g,34 mmol) and methyl
iodide (2 mL,32 mmol).The reaction mixture was stirred overnight
(22 h) after which it was filtered through a glass filter funnel to
remove inorganic salts.The liquids were collected and the solvents
removed under reduced pressure.The solids were then suspended
in 500 mL of chloroform (CHCl3) and extracted with 200 mL of 2
M hydrochloric acid (HCl),200 mL of diluted brine,and finally
200 mL of brine.The organic phase was dried over sodium sulfate
(Na2SO4) and after filtration the solvents were removed and the
product dried under vacuum.The product 6 was isolated in 86%
yield as a yellow solid.The product was a mixture of the
7-methoxycarbonyl derivative and the 8-methoxycarbonyl derivative
in a 3:2 ratio.Major isomer:1H NMR (400 MHz,CDCl3) ä 8.62
(d,J ) 1.7 Hz,1H),8.29 (d,J ) 8.9 Hz,1H),8.23 (dd,J ) 1.7,
8.9 Hz,1H),3.99 (s,3H),3.78 (s,3H),3.56 (s,3H).Minor isomer:
1H NMR (400 MHz,CDCl3) ä 8.92 (d,J ) 1.8 Hz,1H),8.38 (dd,
J ) 1.9,8.9 Hz,1H),7.98 (d,J ) 8.9 Hz),3.97 (s,3H),3.78 (s,
3H),3.56 (s,3H).13C NMR (CDCl3,100 MHz) for the mixture ä
165.7,159.4,159.3,150.5,146.4,145.9,145.3,142.6,141.5,138.9,
134.5,133.3,133.2,131.1,131.0,130.7,

英语翻译Experimental SectionSynthesis of 7/8-Hydroxycarbonylalloxazine (5).To a stirredsolution of 3,4-diaminobenzoic acid (3,3.04 g,20 mmol) in 170mL of acetic acid were added boric acid (1.36 g,22 mmol) andalloxane (4) monohydrate (3.36 g,21 mm
试验段
合成7/8-氢氧根的羰基咯嗪 （ 5 ） .以搅拌
解决3,4 - 二氨基安息香的酸（ 3 ,三点○四克,20 mmol ）在170
毫升乙酸加入硼酸（ 1.36克,22 mmol ）
四氧嘧啶（ 4 ）水合物（三点三六克,21 mmol ） .反应
搅拌3 h后在室温下后,其中沉淀
产品过滤起飞和水洗,首先与乙酸,然后与
乙醚,水,和去年乙醚.该产品5 （绿皮书
粉）被隔离在一个3:2的比例,7 -8 -异构体
定量产量.主要的同分异构体：核磁共振（ 400兆赫,二甲基亚砜的D6 ）
ä 12.02 （ ,为1小时） ,11.79 （ ,为1小时） ,8.29 （四,j ）条1.9赫兹,1小时） ,8.18
（四,j ）条8.8赫兹,1小时） ,8.09 （房屋署副署长,j ）条1.9 ,8.8赫兹,1小时） .轻微的同分异构体：
核磁共振（ 400兆赫,二甲基亚砜- D6中）第12.06 （ ,为1小时） ,11.80 （ ,为1小时） ,
8.55 （四,j ）条2.0赫兹） ,8.25 （房屋署副署长,j ）条2.0 ,8.8赫兹,1小时） ,7.90 （四,j ）条
8.8赫兹,1小时） .13C NMR谱（二甲基亚砜- D6中,100兆赫）为混合ä
167.0 ,167.0 ,160.8 ,160.8 ,150.7 ,150.7 ,148.6 ,148.1 ,145.4 ,142.5 ,
141.4 ,138.8 ,135.1 ,134.0 ,133.7 ,132.8 ,132.5 ,131.1 ,130.8 ,129.1 ,
128.0 ,127.9 .
合成的N1 ,n3-二甲基的-7/8-含甲氧基的羰基咯嗪
（ 6 ） 0.9 ,以搅拌解决7/8-氢氧根的羰基咯嗪 （ 5 ）
（二点五八克,10 mmol ）在500毫升二甲基甲酰胺甲基甲酰胺（ DMF ）
补充说：碳酸钾（碳酸钾） （ 4.70克,34 mmol ）和甲基
碘化物（ 2毫升,32 mmol ） .反应混合物搅拌通宵
（ 22八）后,它通过一个过滤玻璃过滤漏斗
删除无机盐.液体收集和溶剂
删除下减少的压力.固体,然后暂停
在500毫升氯仿（氯仿）和提取200毫升2
米盐酸（ HCL ）中,200毫升稀释卤水,最后
200毫升的盐水.有机相是干超过硫酸钠
（硫酸钠）和过滤后的溶剂被拆除和
产品冻干真空条件下.该产品6月被隔离在86 ％
产量为黄色固体.该产品是一种混合的
7 -甲氧羰基衍生物和8 -甲氧羰基衍生物
在一个3:2的比例.主要的同分异构体：核磁共振（ 400兆赫,cdcl3 ） ä 8.62
（四,j ）条1.7赫兹,1小时） ,8.29 （四,j ）条8.9赫兹,1小时） ,8.23 （房屋署副署长,j ）条1.7 ,
8.9赫兹,1小时） ,3.99 （ ,3小时） ,3.78 （ ,3小时） ,3.56 （ ,3小时） .轻微的同分异构体：
核磁共振（ 400兆赫,cdcl3 ）第8.92 （四,j ）条1.8赫兹,1小时） ,8.38 （房屋署副署长,
j ）条1.9 ,8.9赫兹,1小时） ,7.98 （四,j ）条8.9赫兹） ,3.97 （ ,3小时） ,3.78 （ ,
3小时） ,3.56 （ ,3小时） .13C NMR谱（ cdcl3 ,100兆赫）为混合ä
165.7 ,159.4 ,159.3 ,150.5 ,146.4 ,145.9 ,145.3 ,142.6 ,141.5 ,138.9 ,
134.5 ,133.3 ,133.2 ,131.1 ,131.0 ,130.7

Experimental Section
Synthesis of 7/8-Hydroxycarbonylalloxazine (5). To a stirred
solution of 3,4-diaminobenzoic acid (3, 3.04 g, 20 mmol) in 170
mL of acetic acid were added boric acid...

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Experimental Section
Synthesis of 7/8-Hydroxycarbonylalloxazine (5). To a stirred
solution of 3,4-diaminobenzoic acid (3, 3.04 g, 20 mmol) in 170
mL of acetic acid were added boric acid (1.36 g, 22 mmol) and
alloxane (4) monohydrate (3.36 g, 21 mmol). The reaction was
stirred for 3 h at room temperature after which the precipitated
product was filtered off and washed, first with acetic acid then with
diethyl ether, water, and last diethyl ether. The product 5 (green
powder) was isolated in a 3:2 ratio of the 7- and 8-isomer in
quantitative yield. Major isomer: 1H NMR (400 MHz, DMSOd6)
ä 12.02 (s, 1H), 11.79 (s, 1H), 8.29 (d, J ) 1.9 Hz, 1H), 8.18
(d, J ) 8.8 Hz, 1H), 8.09 (dd, J ) 1.9, 8.8 Hz, 1H). Minor isomer:
1H NMR (400 MHz, DMSO-d6) ä 12.06 (s, 1H), 11.80 (s, 1H),
8.55 (d, J ) 2.0 Hz), 8.25 (dd, J ) 2.0, 8.8 Hz, 1H), 7.90 (d, J )
8.8 Hz, 1H). 13C NMR (DMSO-d6, 100 MHz) for the mixture ä
167.0, 167.0, 160.8, 160.8, 150.7, 150.7, 148.6, 148.1, 145.4, 142.5,
141.4, 138.8, 135.1, 134.0, 133.7, 132.8, 132.5, 131.1, 130.8, 129.1,
128.0, 127.9.
Synthesis of N1,N3-Dimethyl-7/8-methoxycarbonylalloxazine
(6).9 To a stirred solution of 7/8-hydroxycarbonylalloxazine (5)
(2.58 g, 10 mmol) in 500 mL of dimethylformamide (DMF) were
added potassium carbonate (K2CO3) (4.70 g, 34 mmol) and methyl
iodide (2 mL, 32 mmol). The reaction mixture was stirred overnight
(22 h) after which it was filtered through a glass filter funnel to
remove inorganic salts. The liquids were collected and the solvents
removed under reduced pressure. The solids were then suspended
in 500 mL of chloroform (CHCl3) and extracted with 200 mL of 2
M hydrochloric acid (HCl), 200 mL of diluted brine, and finally
200 mL of brine. The organic phase was dried over sodium sulfate
(Na2SO4) and after filtration the solvents were removed and the
product dried under vacuum. The product 6 was isolated in 86%
yield as a yellow solid. The product was a mixture of the
7-methoxycarbonyl derivative and the 8-methoxycarbonyl derivative
in a 3:2 ratio. Major isomer: 1H NMR (400 MHz, CDCl3) ä 8.62
(d, J ) 1.7 Hz, 1H), 8.29 (d, J ) 8.9 Hz, 1H), 8.23 (dd, J ) 1.7,
8.9 Hz, 1H), 3.99 (s, 3H), 3.78 (s, 3H), 3.56 (s, 3H). Minor isomer:
1H NMR (400 MHz, CDCl3) ä 8.92 (d, J ) 1.8 Hz, 1H), 8.38 (dd,
J ) 1.9, 8.9 Hz, 1H), 7.98 (d, J ) 8.9 Hz), 3.97 (s, 3H), 3.78 (s,
3H), 3.56 (s, 3H). 13C NMR (CDCl3, 100 MHz) for the mixture ä
165.7, 159.4, 159.3, 150.5, 146.4, 145.9, 145.3, 142.6, 141.5, 138.9,
134.5, 133.3, 133.2, 131.1, 131.0, 130.7

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