Dichloromethane → HCID 18797021, 화합물

HRID 1003705

반응식

HRID 1003705 반응식
C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[C:15]1([C:21]2[CH:34]=[CH:33][C:24]([C:25]([NH:27][CH2:28][CH2:29][CH2:30][CH:31]=O)=[O:26])=[CH:23][CH:22]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[CH3:35][O:36][C:37]1[CH:46]=[C:45]2[C:40]([CH2:41][CH2:42][NH:43][CH2:44]2)=[CH:39][CH:38]=1.ClCCl>ClCCCl>[CH3:35][O:36][C:37]1[CH:46]=[C:45]2[C:40]([CH2:41][CH2:42][N:43]([CH2:31][CH2:30][CH2:29][CH2:28][NH:27][C:25](=[O:26])[C:24]3[CH:33]=[CH:34][C:21]([C:15]4[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=4)=[CH:22][CH:23]=3)[CH2:44]2)=[CH:39][CH:38]=1

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 4172887-Methoxy-1,2,3,4-TetrahydroisoquinolineHCID 5049666Sodium triacetoxyborohydrideHCID 21712565HCID 21712565, 화합물

생성물 1

HCID 18797021HCID 18797021, 화합물수율 83%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

Sodium triacetoxyborohydride (4.66 g, 22 mmol) was added to a stirred mixture of 4-(4-phenylbenzoylamino)butyraldehyde (3.92 g, 15 mmol) and 7-methoxy-1,2,3,4-tetrahydroisoquinoline [Daniel J. Sall et al., J. Med. Chem., 1987, 30, 2208] (2.40 g, 14.7 mmol) in 1,2-dichloroethane (200 ml) at room temperature. After stirring for 16 h, dichloromethane (100 ml) was added and the mixture was then washed with saturated aqueous K2CO3 (2×100 ml) and brine (100 ml). Drying (Na2SO 4) and evaporation in vacuo afforded a viscous oil which was chromatographed on silica gel, eluting with ethyl acetate, to give the title compound as a pale pink solid (5.04 g, 83%).

후처리

  1. washthe mixture was then washed with saturated aqueous K2CO3 (2×100 ml) and brine (100 ml)
  2. customDrying
  3. custom(Na2SO 4) and evaporation in vacuo
  4. customafforded a viscous oil which
  5. customwas chromatographed on silica gel
  6. washeluting with ethyl acetate

출처 및 근거

ORD 기록
ord-1ec7eec19cdc476f947633e2eee927b0
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06046210

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