Methanol → 6-(Hydroxymethyl)morpholin-3-one

HRID 1048851노트

반응식

HRID 1048851 반응식
CC(C)([O-])C.[K+].Cl[CH2:8][C:9]([NH:11][CH2:12][CH:13]([OH:16])[CH2:14][OH:15])=[O:10].CO.O>C(O)(CC)(C)C>[OH:15][CH2:14][CH:13]1[CH2:12][NH:11][C:9](=[O:10])[CH2:8][O:16]1

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 132331202-Chloro-N-(2,3-dihydroxypropyl)acetamideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 534019466-(Hydroxymethyl)morpholin-3-one수율 91.8%

시약·촉매·용매 1

HCID 64052-Methyl-2-butanol용매2회

실험 절차

To a stirred solution of potassium tert-butoxide (23.4 g, 299.4 mmol) in 200 mL tert-amyl alcohol at room temperature was added 2-chloro-N-(2,3-dihydroxypropyl) acetamide (Step-1 of Intermediate-9) (20 g, 119.6 mmol) in 460 mL tert-amyl alcohol for 2 h under nitrogen atmosphere. After one hour, MeOH (100 mL) and H2O (3 mL) were added and further stirred for 20 min. The reaction mixture was concentrated under vacuum and purified by flash chromatography on silica gel with MeOH/EtOAc (20:80) to give the title compound as a white solid (14.4 g). m/z 132.1

후처리

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. custompurified by flash chromatography on silica gel with MeOH/EtOAc (20:80)

출처 및 근거

ORD 기록
ord-9d567468999448218b4af1949708f0d9
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09382216B2

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