Ammonia → 2-Chloro-1,3-thiazole-5-carboxamide

HRID 747555ノート

反応式

HRID 747555 の反応式
[Cl:1][C:2]1[S:3][C:4]([C:7]([O:9]CC)=O)=[CH:5][N:6]=1.[NH3:12]>CO>[Cl:1][C:2]1[S:3][C:4]([C:7]([NH2:12])=[O:9])=[CH:5][N:6]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 19017727Ethyl 2-chloro-1,3-thiazole-5-carboxylate

生成物 1

HCID 534244962-Chloro-1,3-thiazole-5-carboxamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

Dissolve ethyl 2-chlorothiazole-5-carboxylate (0.927 g, 4.84 mmol) in methanol. Cool the solution to 0° C., then bubble NH3 into the reaction mixture for 10 minutes. Then seal the reaction vessel and stir for 3 hours. Concentrate the reaction mixture to give the title product: 1H NMR (CDCl3): 8.21 (s, 1H), 8.19 (s, 1H), 7.77 (s, 1H); HPLC [YMC-Pro pack C-18 (150×4.6 mm, S-5 microm), 0.05% TFA/acetonitrile in 0.05% TFA/water at 1.0 mL/min, 10-20% over 5 min, 20-95% over 18], tR=6.9 min, 100% purity.

後処理

  1. customThen seal the reaction vessel
  2. concentrationConcentrate the reaction mixture

出典と根拠

ORDレコード
ord-0a6cf79ad19544158e674e2534061340
出典データセット
uspto-grants-2008_07
特許番号
US07396943B2

反応ノート

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