反应 #302921

ord-0425c03deb5f4dd6ad98357a06e309f6

反应方程式

CCOC(=O)Nc1ccsc1C(=O)OC
3-ethoxycarbonylamino-thiophene-2-carboxylic acid methyl ester
NN.O
hydrazine monohydrate
Nn1c(=O)[nH]c2ccsc2c1=O
powder
收率 61.9%
Nn1c(=O)[nH]c2ccsc2c1=O
3-Amino-1H-thieno[3,2-d]pyrimidine-2,4-dione
收率 61.9%

溶剂

反应条件

温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤the mixture was filtered

实验过程

To a solution of 3-ethoxycarbonylamino-thiophene-2-carboxylic acid methyl ester (3.43 g, 15.0 mmol) in EtOH (100 mL) was added hydrazine monohydrate (7.98 mL, 164.6 mmol). After heating at 90° C. for 12 h, the mixture was filtered to afford a fine yellow powder (1.70 g), which was used in the next step without further purification. MS: 184.2. 1H NMR (400 MHz, CD3OD) δ ppm 7.93 (d, J=5.3 Hz, 1H), 6.95 (d, J=5.3 Hz, 1H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08193178B2uspto-grants-2012_06