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

HRID 67776
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HRID 67776 반응식
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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-bf2cde96df4644e89bf9139cab4d6fe7
출처 데이터셋
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04346088

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