Ammonia → 1-(4-(4-chloro-1H-imidazol-1-yl)-3-methoxyphenyl)thiourea

HRID 1803102노트

반응식

HRID 1803102 반응식
[NH3:1].[Cl:2][C:3]1[N:4]=[CH:5][N:6]([C:8]2[CH:13]=[CH:12][C:11]([N:14]=[C:15]=[S:16])=[CH:10][C:9]=2[O:17][CH3:18])[CH:7]=1>>[Cl:2][C:3]1[N:4]=[CH:5][N:6]([C:8]2[CH:13]=[CH:12][C:11]([NH:14][C:15]([NH2:1])=[S:16])=[CH:10][C:9]=2[O:17][CH3:18])[CH:7]=1

참가 물질

3

반응물 2

HCID 222AmmoniaHCID 866498874-chloro-1-(4-isothiocyanato-2-methoxy-phenyl)-1H-imidazole

생성물 1

HCID 866498881-(4-(4-chloro-1H-imidazol-1-yl)-3-methoxyphenyl)thiourea수율 84.6%

실험 절차

Step A (4): Methanolic ammonia (1.0 M, 100 mL, 100 mmol) was added to a flask charged with 4-chloro-1-(4-isothiocyanato-2-methoxy-phenyl)-1H-imidazole (4.27 g, 16.1 mmol) in a ice-water bath. After the addition was complete, the resulting slurry was stirred for 10 min and then allowed to warm to rt. After 24 h, the reaction mixture was concentrated to dryness in vacuo. The solid was suspended in ethanol (200 mL) and stirred for 2 hours. The solid was collected by vacuum filtration and dried under high vacuum for 24 h to afford 1-(4-(4-chloro-1H-imidazol-1-yl)-3-methoxyphenyl)thiourea (3.85 g, 83% yield) as a white solid. LC-MS (M+H)+ 283.0.

후처리

  1. additionAfter the addition
  2. waitAfter 24 h
  3. concentrationthe reaction mixture was concentrated to dryness in vacuo
  4. stirringstirred for 2 hours
  5. filtrationThe solid was collected by vacuum filtration
  6. customdried under high vacuum for 24 h

출처 및 근거

ORD 기록
ord-6c23389b468c4d8aa17b66878dd4a8da
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08349880B2

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