Benzoyl isothiocyanate → HCID 86631119、化合物

HRID 912668ノート

反応式

HRID 912668 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 86631119HCID 86631119、化合物収率 71.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c27561dbf53a493c8a030b4e6d96b91c
出典データセット
uspto-grants-2011_09
特許番号
US08026244B2

反応ノート

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