2-(4-Chlorophenyl)ethylamine → HCID 2780157, 화합물

HRID 879982노트

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HRID 879982 반응식
[N+:1]([C:4]1[C:12]2[S:11][C:10]([C:13]([O:15]CC)=O)=[N+:9]([O-:18])[C:8]=2[CH:7]=[C:6]([C:19]([F:22])([F:21])[F:20])[CH:5]=1)([O-:3])=[O:2].[Cl:23][C:24]1[CH:29]=[CH:28][C:27]([CH2:30][CH2:31][NH2:32])=[CH:26][CH:25]=1>CO>[Cl:23][C:24]1[CH:29]=[CH:28][C:27]([CH2:30][CH2:31][NH:32][C:13]([C:10]2[S:11][C:12]3[C:4]([N+:1]([O-:3])=[O:2])=[CH:5][C:6]([C:19]([F:21])([F:22])[F:20])=[CH:7][C:8]=3[N+:9]=2[O-:18])=[O:15])=[CH:26][CH:25]=1

참가 물질

4

반응물 2

HCID 674302-(4-Chlorophenyl)ethylamineHCID 2779933HCID 2779933, 화합물

생성물 1

HCID 2780157HCID 2780157, 화합물수율 60.5%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
25 °C

실험 절차

A suspension of 0.3 g (0.89 mmol) of ethyl 7-nitro-5-(trifluoromethyl)-1,3-benzothiazole-2-carboxylate-3-oxide (the synthesis of which is described in Wagner et al., Chem. Ber., 1973, 106, 640-654 compound 4e and Bayer patent DE 2013434, example 7), in 9 ml of methanol is heated with stirring until solubilization, and then cooled to 25° C. 0.157 g (1.01 mmol) of 2-(4-chlorophenyl)ethanamine is added slowly to the solution obtained. The homogeneous reaction mixture is stirred at AT overnight. It is then concentrated under reduced pressure and the residue obtained is purified by silica column chromatography (solvent: cyclohexane/-dichloromethane from 60/40 to 0/100). 0.240 g of expected compound is obtained.

후처리

  1. customthe synthesis of which
  2. temperatureis heated
  3. customobtained
  4. stirringThe homogeneous reaction mixture is stirred at AT overnight
  5. concentrationIt is then concentrated under reduced pressure
  6. customthe residue obtained
  7. customis purified by silica column chromatography (solvent: cyclohexane/-dichloromethane from 60/40 to 0/100)

출처 및 근거

ORD 기록
ord-d91438bf270b45ae977323b3726d608e
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993561B2

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