(1-Bromoethyl)benzene → HCID 178463349, 화합물

HRID 502795노트

반응식

HRID 502795 반응식
[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

참가 물질

4

반응물 2

HCID 11454(1-Bromoethyl)benzeneHCID 178508009HCID 178508009, 화합물

생성물 1

HCID 178463349HCID 178463349, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-618a244c729840fa9bdca0abad939ede
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776878B2

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