Ammonia → HCID 178431879、化合物

HRID 588746

反応式

HRID 588746 の反応式
[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

参加物

6

反応物 4

HCID 222AmmoniaHCID 6213Dimethyl SulfoneHCID 521132Ethyl 2-amino-4-methylthiophene-3-carboxylateHCID 3084509Chloroformamidinium chloride

生成物 1

HCID 178431879HCID 178431879、化合物収率 87.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
135 °C

実験手順

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]+.

後処理

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

出典と根拠

ORDレコード
ord-c1695a9815aa42c2b10daecd926f3082
出典データセット
uspto-grants-2016_01
特許番号
US09227984B2

関連ノート

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