Ammonia → 1-(3-methoxy-4-(1-methyl-1H-pyrazol-4-yl)phenyl)thiourea

HRID 1803145노트

반응식

HRID 1803145 반응식
[NH3:1].[N:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]=[N:13][N:14]([CH3:16])[CH:15]=2)=[C:7]([O:17][CH3:18])[CH:6]=1)=[C:3]=[S:4]>>[CH3:18][O:17][C:7]1[CH:6]=[C:5]([NH:2][C:3]([NH2:1])=[S:4])[CH:10]=[CH:9][C:8]=1[C:11]1[CH:12]=[N:13][N:14]([CH3:16])[CH:15]=1

참가 물질

3

반응물 2

HCID 222AmmoniaHCID 866499074-(4-isothiocyanato-2-methoxyphenyl)-1-methyl-1H-pyrazole

생성물 1

HCID 866499081-(3-methoxy-4-(1-methyl-1H-pyrazol-4-yl)phenyl)thiourea수율 86.5%

실험 절차

Step K (4): Methanolic ammonia (2.0 M, 20 mL, 40 mmol) was added to a flask charged with 4-(4-isothiocyanato-2-methoxyphenyl)-1-methyl-1H-pyrazole (1.46 g, 5.95 mmol). After 3 h, the reaction mixture was concentrated in vacuo. The solid was triturated with diethyl ether. The solid was collected by vacuum filtration and dried under high vacuum to afford 1-(3-methoxy-4-(1-methyl-1H-pyrazol-4-yl)phenyl)thiourea (1.35 g, 86% yield). LC-MS (M+H)+ 263.1.

후처리

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. customThe solid was triturated with diethyl ether
  3. filtrationThe solid was collected by vacuum filtration
  4. customdried under high vacuum

출처 및 근거

ORD 기록
ord-1867edefc8ae481fa0338eba781a3c70
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08349880B2

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