Hydrochloric Acid → 3-((3-(10,11-Dihydro-5h-dibenz[b,f]azepin-5-yl)-1-propyl)amino)benzoic acid

HRID 1737226

반응식

HRID 1737226 반응식
C([O:3][C:4](=[O:33])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([N:11](C(=O)C)[CH2:12][CH2:13][CH2:14][N:15]2[C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=3[CH2:19][CH2:18][C:17]3[CH:26]=[CH:27][CH:28]=[CH:29][C:16]2=3)[CH:6]=1)C.O.Cl>C(O)C.[OH-].[Na+]>[CH:26]1[C:17]2[CH2:18][CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[N:15]([CH2:14][CH2:13][CH2:12][NH:11][C:7]3[CH:6]=[C:5]([CH:10]=[CH:9][CH:8]=3)[C:4]([OH:33])=[O:3])[C:16]=2[CH:29]=[CH:28][CH:27]=1

참가 물질

6

실험 절차

To a solution of the above ester (1.0 g, 0.0023 mol) in ethanol (5 ml), 4N sodium hydroxide (0.6 ml) was added and the mixture was stirred at room temperature for 6 h and then left in a freezer overnight. The reaction mixture was allowed to warm up to room temperature and additional 4N sodium hydroxide (0.6 ml) was added. The mixture was stirred at room temperature for 3 h. Water and 4N hydrochloric acid (1.7 ml) were added, and the mixture was extracted with dichloromethane (2×200 ml). The combined organic extracts were dried (MgSO4) and the solvent was evaporated in vacuo. The residue was stripped twice with dichloromethane and dried in vacuo affording 0.5 g (59%) of the title compound as an amorphous solid.

후처리

  1. waitleft in a freezer overnight
  2. temperatureto warm up to room temperature
  3. stirringThe mixture was stirred at room temperature for 3 h
  4. extractionthe mixture was extracted with dichloromethane (2×200 ml)
  5. dry with materialThe combined organic extracts were dried (MgSO4)
  6. customthe solvent was evaporated in vacuo
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-2cb4303f53234788b95a9f888662186b
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05962449

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