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N-Methylbenzylamine → HCID 19968859, 화합물

HRID 976100
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HRID 976100 반응식
Cl[CH2:2][CH2:3][CH:4]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:5]([N:7]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)=[O:6].[CH3:20][NH:21][CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.C(N(C(C)C)CC)(C)C>C(#N)C>[CH2:22]([N:21]([CH2:2][CH2:3][CH:4]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:5]([N:7]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)=[O:6])[CH3:20])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7669N-MethylbenzylamineHCID 81531DiisopropylethylamineHCID 152860151-Azepan-1-yl-4-chloro-2-phenylbutan-1-one

생성물 1

HCID 19968859HCID 19968859, 화합물수율 57.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

A solution of 2,3,4,5,6,7-hexahydro-1-[4-chloro-2-phenylbutanoyl]-1H-azepine (10.0 g, 35.7 mmol) in acetonitrile (100 ml) was added to a solution of N-methylbenzylamine (4.03 g, 33.3 mmol) and diisopropylethylamine (4.62 g, 35.7 mmol) in acetonitrile (40 ml) and the reaction mixture stirred at room temperature overnight. The reaction mixture was concentrated under reduced pressure and the residue dissolved in water (100 ml). The aqueous phase was washed with ethyl acetate (3×50 ml) and the combined organic phases washed with brine (50 ml), water (50 ml), dried (MgSO4) and concentrated under reduced pressure. The crude oil obtained was chromatographed on alumina, eluting with hexane:ethyl acetate (2:1) to afford the title compound as an oil (6.93 g, 53%).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe residue dissolved in water (100 ml)
  3. washThe aqueous phase was washed with ethyl acetate (3×50 ml)
  4. washthe combined organic phases washed with brine (50 ml), water (50 ml)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure
  7. customThe crude oil obtained
  8. customwas chromatographed on alumina
  9. washeluting with hexane:ethyl acetate (2:1)

출처 및 근거

ORD 기록
ord-8d3699bec7e54788bbd8a59fe3272bfe
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05610295

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