HCID 22292777、化合物 → HCID 22292795、化合物

HRID 881938ノート

反応式

HRID 881938 の反応式
[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]

参加物

5

反応物 2

HCID 22292777HCID 22292777、化合物HCID 178418546HCID 178418546、化合物

生成物 1

HCID 22292795HCID 22292795、化合物収率 64%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4a3404c70cfc4e06a406e12f2478713a
出典データセット
uspto-grants-2015_03
特許番号
US08993750B2

反応ノート

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