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Methylamine → 4-(4-Chloro-3-methylsulfamoylphenyl)-2-(4-methoxyphenylimino)-3-methyl-4-thiazoline hydrochloride

HRID 67776
ノート
印刷プレビュー

反応式

HRID 67776 の反応式
Br.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2(O)[CH2:13][S:12][C:11](=[N:14][C:15]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=3)[N:10]2[CH3:23])=[CH:5][C:4]=1[S:25](Cl)(=[O:27])=[O:26].[CH3:29][NH2:30]>CO>[ClH:2].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]([CH3:23])[C:11](=[N:14][C:15]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=3)[S:12][CH:13]=2)=[CH:5][C:4]=1[S:25](=[O:27])(=[O:26])[NH:30][CH3:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6329MethylamineHCID 867385554-(4-Chloro-3-chlorosulfonylphenyl)-2-(4-methoxyphenyl-imino)-3-methylthiazolidin-4-ol hydrobromide

生成物 1

HCID 205271204-(4-Chloro-3-methylsulfamoylphenyl)-2-(4-methoxyphenylimino)-3-methyl-4-thiazoline hydrochloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

10.6 g (0.02 mole) of 4-(4-chloro-3-chlorosulfonylphenyl)-2-(4-methoxyphenyl-imino)-3-methylthiazolidin-4-ol hydrobromide are introduced into a mixture of 10 ml of 40% strength aqueous methylamine and 150 ml of methanol and the resulting mixture is stirred for 20 hours at room temperature. The solvent is distilled off, the residue is taken up in 100 ml of ethanol and this solution is acidified with methanolic or ethanolic hydrogen chloride solution and heated at the boil for 2 hours. The solvent is distilled off, the residue is crystallized under ether, ethyl acetate or diisopropyl ether and the crystals are filtered off. Melting point 257° C. (with decomposition) (from isopropanol).

後処理

  1. distillationThe solvent is distilled off
  2. temperatureheated at the boil for 2 hours
  3. distillationThe solvent is distilled off
  4. customthe residue is crystallized under ether
  5. filtrationethyl acetate or diisopropyl ether and the crystals are filtered off

出典と根拠

ORDレコード
ord-bf2cde96df4644e89bf9139cab4d6fe7
出典データセット
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04346088

反応ノート

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