2-(1H-imidazol-1-yl)ethanamine → HCID 178477864, 화합물

HRID 580863

반응식

HRID 580863 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[C:8](=S)[NH:7][C:6]=2[CH:17]=1.[NH2:18][CH2:19][CH2:20][N:21]1[CH:25]=[CH:24][N:23]=[CH:22]1>C(OCCO)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[C:8]([NH:18][CH2:19][CH2:20][N:21]3[CH:25]=[CH:24][N:23]=[CH:22]3)=[N:7][C:6]=2[CH:17]=1

참가 물질

4

반응물 2

HCID 4306672-(1H-imidazol-1-yl)ethanamineHCID 125357788-Chloro-5,10-dihydro-dibenzo[b,e][1,4]diazepin-11-thione

생성물 1

HCID 178477864HCID 178477864, 화합물수율 57.1%

시약·촉매·용매 1

HCID 8076Glycol monoethyl ether용매

실험 절차

A solution of 0.6 g (2.3 mmol) of 8-chloro-5,10-dihydro-dibenzo[b,e][1,4]diazepin-11-thione in 15 mL of 2-ethoxyethanol was treated with 0.6 mL (4.6 mmol) of 1-(2-aminoethyl)imidazole and heated at reflux for 2 days. The solvent was removed under reduced pressure and the residue taken up in EtOAc and washed three times with H2O, then saturated NaHCO3 solution, and saturated NaCl solution. Drying over MgSO4 and removal of the solvent under reduced pressure left the crude product. This was recrystallized from EtOAc/hexane using charcoal to give 0.44 g (57.1% yield) of the product as pale yellow crystals, mp 168-170° C. The structure was confirmed by NMR and mass spectroscopy. (m+H)+ =338.

후처리

  1. temperatureheated
  2. temperatureat reflux for 2 days
  3. customThe solvent was removed under reduced pressure
  4. washwashed three times with H2O
  5. dry with materialDrying over MgSO4 and removal of the solvent under reduced pressure
  6. waitleft the crude product
  7. customThis was recrystallized from EtOAc/hexane

출처 및 근거

ORD 기록
ord-5b925a6dbad44516b076de80e86a116d
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05919780

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