4-Fluorophenyl isothiocyanate → HCID 86662261, 화합물

HRID 1627397노트

반응식

HRID 1627397 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([CH3:17])([CH3:16])[C:12]([NH:14][NH2:15])=[O:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[F:18][C:19]1[CH:24]=[CH:23][C:22]([N:25]=[C:26]=[S:27])=[CH:21][CH:20]=1>CCO>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([CH3:17])([CH3:16])[C:12]([NH:14][NH:15][C:26](=[S:27])[NH:25][C:22]2[CH:23]=[CH:24][C:19]([F:18])=[CH:20][CH:21]=2)=[O:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

참가 물질

4

반응물 2

HCID 152414-Fluorophenyl isothiocyanateHCID 66740370HCID 66740370, 화합물

생성물 1

HCID 86662261HCID 86662261, 화합물수율 72%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 2-(3,4-dimethoxyphenyl)-2-methylpropanehydrazide (1.04 g, 4.37 mmol) and 4-fluorophenyl isothiocyanate (1.34 g, 8.73 mmol) in EtOH (30 mL) was heated at reflux 2 h. The reaction mixture was cooled and filtered. The filtrate was concentrated in vacuo and the residue was triturated with Et2O. The solids were collected by filtration and dried in vacuo to give 2-(2-(3,4-dimethoxyphenyl)-2-methylpropanoyl)-N-(4-fluorophenyl)hydrazinecarbothioamide (1.23 g, 72%). 1H NMR (400 MHz, DMSO-d6) δ 9.70 (br s, 1H), 9.65 (br s, 1H), 7.38 (b, 1H), 7.17 (t, 3H), 6.94-6.82 (m, 4H), 3.73 (s, 3H), 3.71 (s, 3H), 1.52 (s, 6H).

후처리

  1. temperaturewas heated
  2. temperatureat reflux 2 h
  3. temperatureThe reaction mixture was cooled
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated in vacuo
  6. customthe residue was triturated with Et2O
  7. filtrationThe solids were collected by filtration
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-8e998b9c7b8a4ec2a93796aca0363281
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785488B2

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