N-bromobutanimide → HCID 178419416、化合物

HRID 1851302ノート

反応式

HRID 1851302 の反応式
[C:1]1([C:7]2[C:8]([C:16]3[CH:21]=[CH:20][C:19]([CH2:22][N:23]4[CH2:26][CH:25]([C:27]5[N:31]=[C:30]([C:32]6[CH:37]=[CH:36][CH:35]=[CH:34][N:33]=6)[NH:29][N:28]=5)[CH2:24]4)=[CH:18][CH:17]=3)=[N:9][C:10]3[N:11]([CH:13]=[CH:14][N:15]=3)[CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Br:38]N1C(=O)CCC1=O>C(Cl)(Cl)Cl>[Br:38][C:13]1[N:11]2[CH:12]=[C:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[C:8]([C:16]3[CH:21]=[CH:20][C:19]([CH2:22][N:23]4[CH2:24][CH:25]([C:27]5[N:31]=[C:30]([C:32]6[CH:37]=[CH:36][CH:35]=[CH:34][N:33]=6)[NH:29][N:28]=5)[CH2:26]4)=[CH:18][CH:17]=3)=[N:9][C:10]2=[N:15][CH:14]=1

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 178420104HCID 178420104、化合物

生成物 1

HCID 178419416HCID 178419416、化合物収率 11.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

143 mg (0.3 mmol) 6-Phenyl-7-{4-{3-[5-(pyridine-2-yl)-1H-[1,2,4]triazole-3-yl)azetidine-1-ylmethyl]-phenyl}-imidazo[1,2-a]pyrimidine are dissolved in 11.8 mL chloroform. 57.8 mg (0.3 mmol) N-bromosuccinimide are added and the reaction mixture is heated for one hour at reflux. The solvent is evaporated and the residue is purified by chromatography (silicagel, eluents: dichloromethane/methanol). 19.1 mg (10%) pure compound and 75.8 mg (41%) slightly contaminated product are obtained.

後処理

  1. temperaturethe reaction mixture is heated for one hour
  2. temperatureat reflux
  3. customThe solvent is evaporated
  4. customthe residue is purified by chromatography (silicagel, eluents: dichloromethane/methanol)

出典と根拠

ORDレコード
ord-efbce9e9b9434544b4849b4a6ff2c79b
出典データセット
uspto-grants-2015_02
特許番号
US08957064B2

反応ノート

読み込み中…