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Triethylamine → HCID 19389481, 화합물

HRID 1757049
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HRID 1757049 반응식
[Si:1]([O:8][CH2:9][CH:10]1[O:15][C:14](=[O:16])[CH2:13][CH:12](O)[CH2:11]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C(N(CC)CC)C.CS(Cl)(=O)=O>ClCCl>[Si:1]([O:8][CH2:9][CH:10]1[O:15][C:14](=[O:16])[CH:13]=[CH:12][CH2:11]1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 19389468HCID 19389468, 화합물

생성물 1

HCID 19389481HCID 19389481, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
-50 °C

실험 절차

To 6-t-butyldimethylsilyloxymethyl-4-hydroxytetrahydropyran-2-one (0.52 parts) in dichloromethane (40 parts) was added triethylamine (0.8 parts) and the solution was cooled to -50° C. To this solution was then added a solution of methanesulphonyl chloride (0.48 parts) in dichloromethane (8 parts) during a period of one minute. The reaction mixture was then stirred for 30 minutes at -50° C. before warming to ambient temperature. After a further 3 hours the solution was washed with water, dried over magnesium sulphate and evaporated to obtain 6-t-butyldimethylsilyloxymethyl-5,6-dihydropyran-2-one (0.4 parts).

후처리

  1. temperaturebefore warming to ambient temperature
  2. washAfter a further 3 hours the solution was washed with water
  3. dry with materialdried over magnesium sulphate
  4. customevaporated

출처 및 근거

ORD 기록
ord-dd11cc5f47cc41ea99a0b7448f66275f
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05443970

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