Water → HCID 178487709, 화합물

HRID 420066노트

반응식

HRID 420066 반응식
[CH:1]([C:4]1[CH:8]=[CH:7][NH:6][N:5]=1)([CH3:3])[CH3:2].Cl[C:10]1[CH:19]=[C:18]([O:20]CC2C=CC(OC)=CC=2)[C:17]2[C:12](=[C:13]([CH3:32])[C:14]([O:30][CH3:31])=[CH:15][CH:16]=2)[N:11]=1.O>CN1CCCC1=O>[OH:20][C:18]1[C:17]2[C:12](=[C:13]([CH3:32])[C:14]([O:30][CH3:31])=[CH:15][CH:16]=2)[N:11]=[C:10]([N:6]2[CH:7]=[CH:8][C:4]([CH:1]([CH3:3])[CH3:2])=[N:5]2)[CH:19]=1

참가 물질

5

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HCID 962WaterHCID 566051592-Chloro-8-methyl-7-methoxy-4-(4-methoxy-benzyloxy)-quinolineHCID 178439403HCID 178439403, 화합물

생성물 1

HCID 178487709HCID 178487709, 화합물수율 49%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

A solution of compound 86b (350 mg, 1 eq.) and compound 46b (480 mg, 6 eq.) in N-methylpyrrolidone (5 mL) was heated at 200° C. for 30 min. After the reaction mixture was cooled to room temperature, water was added. The mixture was extracted with EtOAc, dried over Na2SO4, filtered, and concentrated under reduced pressure. The crude material was purified by chromatography on silica gel (EtOAc/DCM). Recrystallisation in diethylether gave compound 88b as a white solid in 49% yield.

후처리

  1. extractionThe mixture was extracted with EtOAc
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe crude material was purified by chromatography on silica gel (EtOAc/DCM)
  6. customRecrystallisation in diethylether

출처 및 근거

ORD 기록
ord-0c381fc0261441bab9403921aca5552a
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093379B2

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