Triethylamine → 1,3-Dimethoxypropan-2-yl methanesulfonate

HRID 636941

반응식

HRID 636941 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][O:7][CH2:8][CH:9]([OH:13])[CH2:10][O:11][CH3:12].C(N(CC)CC)C>ClCCl>[CH3:6][O:7][CH2:8][CH:9]([O:13][S:2]([CH3:1])(=[O:4])=[O:3])[CH2:10][O:11][CH3:12]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 121901,3-Dimethoxy-2-propanolHCID 31297Methanesulfonyl chloride

생성물 1

HCID 225957861,3-Dimethoxypropan-2-yl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4.3 mL of methanesulfonyl chloride was added dropwise at 5° C. to a stirred solution of 6.0 g of 1,3-dimethoxy-propan-2-ol and 9.0 mL of triethylamine in 60 mL of dichloromethane. Stirring was continued for 72 hours at room temperature, followed by extraction with water. The combined organic extracts were dried (sodium sulfate) and concentrated and the residue purified by silica chromatography (isohexane/ethyl acetate=9/1, 8/2, 7/3, 6/4 v/v) yielding 2.5 g of methanesulfonic acid 2-methoxy-1-methoxymethyl-ethyl ester as an oil. EI-MS: 198 (M+).

후처리

  1. extractionfollowed by extraction with water
  2. dry with materialThe combined organic extracts were dried (sodium sulfate)
  3. concentrationconcentrated
  4. customthe residue purified by silica chromatography (isohexane/ethyl acetate=9/1, 8/2, 7/3, 6/4 v/v)

출처 및 근거

ORD 기록
ord-4da37c10c8764a82852b00f406176c90
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194409B1

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