(1-Bromoethyl)benzene → HCID 178463349、化合物

HRID 502795ノート

反応式

HRID 502795 の反応式
[C:1]1([C:7]2[NH:16][C:10]3=[N:11][CH:12]=[C:13]([NH2:15])[CH:14]=[C:9]3[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:17]1([CH:23](Br)[CH3:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>CN(C)C=O>[C:17]1([CH:23]([NH:15][C:13]2[CH:14]=[C:9]3[N:8]=[C:7]([C:1]4[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=4)[NH:16][C:10]3=[N:11][CH:12]=2)[CH3:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

4

反応物 2

HCID 11454(1-Bromoethyl)benzeneHCID 178508009HCID 178508009、化合物

生成物 1

HCID 178463349HCID 178463349、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

100 mg 2-phenyl-3H-imidazo[4,5-b]pyridin-6-ylamine from ex. b) were dissolved in 1 mL dry dimethylformamide (DMF) and 92 mg 1-phenylethyl bromide were added at room temperature. The mixture was stirred for 18 hours (hrs), the DMF was removed under vacuum and the residue purified by chromatography on silica eluting stepwise first with dichloromethane, then dichloromethane/methanol (60:1), then dichloromethane/methanol/ammonia (60:1:0,2). Product containing fractions were pooled and further purified by preparative HPLC-MS.

後処理

  1. customthe DMF was removed under vacuum
  2. customthe residue purified by chromatography on silica eluting stepwise first with dichloromethane
  3. additionProduct containing fractions
  4. customfurther purified by preparative HPLC-MS

出典と根拠

ORDレコード
ord-618a244c729840fa9bdca0abad939ede
出典データセット
uspto-grants-2010_08
特許番号
US07776878B2

反応ノート

読み込み中…