Methanol → 4-(3,4-Dimethoxyphenyl)-2-(2-hydroxyethyl)-6,7-dimethoxyquinazoline

HRID 1458930노트

반응식

HRID 1458930 반응식
CO.[CH3:3][O:4][C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][C:14]=1[O:15][CH3:16])[N:11]=[C:10]([CH2:17][C:18](OC)=[O:19])[N:9]=[C:8]2[C:22]1[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[C:24]([O:30][CH3:31])[CH:23]=1.[BH4-].[Na+].O1CCCC1>O>[CH3:3][O:4][C:5]1[CH:6]=[C:7]2[C:12](=[CH:13][C:14]=1[O:15][CH3:16])[N:11]=[C:10]([CH2:17][CH2:18][OH:19])[N:9]=[C:8]2[C:22]1[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[C:24]([O:30][CH3:31])[CH:23]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 4311764Sodium borohydrideHCID 212240726,7-Dimethoxy-4-(3,4-dimethoxyphenyl)quinazoline-2-acetic acid methyl ester

생성물 1

HCID 220975944-(3,4-Dimethoxyphenyl)-2-(2-hydroxyethyl)-6,7-dimethoxyquinazoline수율 81%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Methanol (15 ml) was added dropwise under reflux to a mixture of methyl 6,7-dimethoxy-4-(3,4-dimethoxyphenyl)-quinazoline-2-acetate (4.0 g), sodium borohydride (1.9 g) and tetrahydrofuran (80 ml). The mixture was stirred under reflux for 2 hours, poured into water and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over magnesium sulfate. The solvent was evaporated under reduced pressure to give 6,7-dimethoxy-4-(3,4-dimethoxyphenyl)-2-(2-hydroxyethyl)quinazoline (3.0 g, 81%) which was then recrystallized from ethyl acetate. Colorless needle crystals. mp. 165°-166° C.

후처리

  1. temperatureunder reflux for 2 hours
  2. extractionextracted with ethyl acetate
  3. washThe ethyl acetate layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-522738c713d74fb29cb05309b02f1e02
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05852039

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