Methanol → HCID 15062404, 화합물

HRID 486849노트

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HRID 486849 반응식
CC1(C)O[C:6](=[O:8])[CH:5]=[C:4]([CH2:9][CH:10]([OH:13])[CH2:11][Cl:12])[O:3]1.C(=O)([O-])[O-].[K+].[K+].CO>C(OCC)(=O)C>[Cl:12][CH2:11][CH:10]1[O:13][C:6](=[O:8])[CH2:5][C:4](=[O:3])[CH2:9]1

참가 물질

5

반응물 3

HCID 887Methanol2회HCID 11430Potassium CarbonateHCID 14944829HCID 14944829, 화합물

생성물 1

HCID 15062404HCID 15062404, 화합물수율 74%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 940 mg (4.26 mmol) of (-)-2,2-dimethyl-6-(3-chloro-2-hydroxypropyl)-1,3-dioxin-4-one (98% ee), 882 mg (6.39 mmol) of potassium carbonate and 10 ml of methanol was stirred at room temperature for 12 hours. After completion of the reaction, methanol was distilled off, and the resultant residue was neutralized with 10% HCl and then extracted with ethyl acetate, followed by drying over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was subjected to column chromatography (an eluent of hexane:ethyl acetate=3:1), thereby obtaining 510 mg (yield 74%) of (-)-6-chloromethyltetrahydropyran-2,4-dione.

후처리

  1. distillationwas distilled off
  2. extractionextracted with ethyl acetate
  3. dry with materialby drying over anhydrous magnesium sulfate
  4. distillationAfter the solvent was distilled off

출처 및 근거

ORD 기록
ord-118aa606c6fb42efbeefd59031e5a285
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292891

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