氨 → HCID 178431879，化合物

HRID 588746

反应方程式

HRID 588746 反应方程式
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH3:12])[C:6]=1[C:7](OCC)=[O:8].Cl.Cl[C:15]([NH2:17])=[NH:16].CS(C)(=O)=O.N>O>[NH2:17][C:15]1[NH:1][C:2]2[S:3][CH:4]=[C:5]([CH3:12])[C:6]=2[C:7](=[O:8])[N:16]=1

参与物

6

反应物 4

HCID 222氨HCID 6213二甲基砜HCID 5211322-氨基-4-甲基-噻吩-3-羧酸乙酯HCID 3084509氯甲脒盐酸盐

产物 1

HCID 178431879HCID 178431879，化合物收率 87.9%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
135 °C

实验过程

A mixture of ethyl 2-amino-4-methylthiophene-3-carboxylate (2.0 g, 11.7 mmol), chloroformamidine hydrochloride (3.357 g, 29.0 mmol) and dimethylsulfone (5.489 g, 58.4 mmol) was heated at 135° C. for 45 minutes. Water was added and the mixture was cooled down to room temperature. An aqueous ammonia solution was added to adjust the solution to pH 9. The precipitate was filtered off, yielding the title compound (1.863 g) as a white powder. 13C NMR δ (75 MHz, DMSO-d6) 168.98, 159.12, 153.21, 133.26, 114.37, 110.81, 16.35. MS (m/z) 182 [M+H]+.

后处理

  1. temperaturethe mixture was cooled down to room temperature
  2. filtrationThe precipitate was filtered off

来源与证据

ORD记录
ord-c1695a9815aa42c2b10daecd926f3082
来源数据集
uspto-grants-2016_01
专利号
US09227984B2

关联笔记

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