HCID 22292777, 화합물 → HCID 22292795, 화합물

HRID 881938노트

반응식

HRID 881938 반응식
[F:1][C:2]([F:21])([F:20])[C:3]([N:5]1[CH2:11][CH:10]([CH3:12])[C:9]2[CH:13]=[C:14](Br)[C:15]([O:17][CH3:18])=[CH:16][C:8]=2[CH2:7][CH2:6]1)=[O:4].[C:22]([Cu])#[N:23]>CN(C)C=O.O>[F:1][C:2]([F:21])([F:20])[C:3]([N:5]1[CH2:11][CH:10]([CH3:12])[C:9]2[CH:13]=[C:14]([C:22]#[N:23])[C:15]([O:17][CH3:18])=[CH:16][C:8]=2[CH2:7][CH2:6]1)=[O:4]

참가 물질

5

반응물 2

HCID 22292777HCID 22292777, 화합물HCID 178418546HCID 178418546, 화합물

생성물 1

HCID 22292795HCID 22292795, 화합물수율 64%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A solution of N-trifluoroacetyl-8-bromo-7-methoxy-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine (18 mg, 0.05 mmol) in dimethylformamide (1 mL) was treated with CuCN (20 mg, 0.24 mmol) and the mixture was microwaved at 200 C for 0.5 hours. The product mixture was diluted with water (5 mL), extracted twice with EtOAc (5 mL), the is combined organic phases were washed with brine (5 mL), dried with Na2SO4 and concentrated. Flash chromatography (35% EtOAc in hexane, silica) resulted in 10 mg of a clear oil. MS calculated for C15H15F3N2O2+H: 313, observed: 313.

후처리

  1. customthe mixture was microwaved at 200 C for 0.5 hours
  2. extractionextracted twice with EtOAc (5 mL)
  3. washwere washed with brine (5 mL)
  4. dry with materialdried with Na2SO4
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4a3404c70cfc4e06a406e12f2478713a
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993750B2

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