Benzoyl isothiocyanate → HCID 86631119, 화합물

HRID 912668노트

반응식

HRID 912668 반응식
Cl.Cl.[NH:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[N:5]=[C:4]1[CH:12]([NH2:14])[CH3:13].CCN(C(C)C)C(C)C.C([N:32]=[C:33]=[S:34])(=O)C1C=CC=CC=1>C(Cl)Cl>[NH:3]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[N:5]=[C:4]1[CH:12]([NH:14][C:33]([NH2:32])=[S:34])[CH3:13]

참가 물질

5

반응물 3

HCID 68284Benzoyl isothiocyanateHCID 81531DiisopropylethylamineHCID 173254751-(1H-Benzoimidazol-2-yl)-ethylamine

생성물 1

HCID 86631119HCID 86631119, 화합물수율 71.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of 1-(1H-Benzoimidazol-2-yl)-ethylamine dihydrochloride (0.50 g, 2.1 mmol) in CH2Cl2 (10 mL) was added DIPEA (0.74 mL, 4.3 mmol). After 5 minutes benzoyl isothiocyanate (0.32 mL, 2.4 mmol) was added and the reaction mixture was stirred for 2.5 h, followed by evaporation in vacuo. Ammonia (7M in MeOH, 20 mL) was then added and the reaction was stirred another 2.5 h. The excess ammonia was removed in vacuo and CH2Cl2 (10 mL) was added, the solid was collected by filtration giving the title compound (0.33 g, 70%). MS (ESI) m/z 221 (M+1).

후처리

  1. customfollowed by evaporation in vacuo
  2. additionAmmonia (7M in MeOH, 20 mL) was then added
  3. stirringthe reaction was stirred another 2.5 h
  4. customThe excess ammonia was removed in vacuo and CH2Cl2 (10 mL)
  5. additionwas added
  6. filtrationthe solid was collected by filtration

출처 및 근거

ORD 기록
ord-c27561dbf53a493c8a030b4e6d96b91c
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026244B2

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