4-Bromophenacyl bromide → HCID 89826358、化合物

HRID 2272959ノート

反応式

HRID 2272959 の反応式
C(=O)([O-])[O-].[K+].[K+].[NH:7]1[CH:11]=[CH:10][CH:9]=[C:8]1[C:12]#[N:13].Br[CH2:15][C:16]([C:18]1[CH:23]=[CH:22][C:21]([Br:24])=[CH:20][CH:19]=1)=[O:17]>CN(C=O)C.ClCCl>[Br:24][C:21]1[CH:22]=[CH:23][C:18]([C:16](=[O:17])[CH2:15][N:7]2[CH:11]=[CH:10][CH:9]=[C:8]2[C:12]#[N:13])=[CH:19][CH:20]=1

参加物

6

反応物 3

HCID 74544-Bromophenacyl bromideHCID 11430Potassium CarbonateHCID 138277Pyrrole-2-carbonitrile

生成物 1

HCID 89826358HCID 89826358、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

5.53 g (40.0 mmol) Potassium carbonate is added to a solution of 1.70 ml (20.0 mmol) pyrrole-2-carbonitrile and 8.34 g (30.0 mmol) 2,4′-dibromoacetophenone in 40 ml DMF. The resulting suspension is stirred for 1 hour at room temperature. The reaction mixture is diluted with dichloromethane and filtered with suction. The residue is washed with dichloromethane. The filtrate is evaporated and the residue is chromatographed on a silica gel column with cyclohexane/ethyl acetate as eluent to give 1-[2-(4-bromo-phenyl)-2-oxo-ethyl]-1H-pyrrole-2-carbonitrile as light orange solid; HPLC/MS 2.80 (B), [M+H] 289/291.

後処理

  1. filtrationfiltered with suction
  2. washThe residue is washed with dichloromethane
  3. customThe filtrate is evaporated
  4. customthe residue is chromatographed on a silica gel column with cyclohexane/ethyl acetate as eluent

出典と根拠

ORDレコード
ord-a914ffa5054949d3b1bab44b8892ff90
出典データセット
uspto-grants-2015_09
特許番号
US09120805B2

反応ノート

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