Triethylamine → 4-(Methanesulfonyl)oxytetrahydrothiopyran

HRID 2270104노트

반응식

HRID 2270104 반응식
[OH:1][CH:2]1[CH2:7][CH2:6][S:5][CH2:4][CH2:3]1.[CH3:8][S:9](Cl)(=[O:11])=[O:10].C(N(CC)CC)C>C(Cl)Cl>[CH3:8][S:9]([O:1][CH:2]1[CH2:7][CH2:6][S:5][CH2:4][CH2:3]1)(=[O:11])=[O:10]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 576296Tetrahydro-2H-thiopyran-4-ol

생성물 1

HCID 124202654-(Methanesulfonyl)oxytetrahydrothiopyran

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a 300 ml methylene chloride solution of 14.6 g (0.12 mol) of 4-hydroxytetrahydrothiopyran, 11.5 ml (0.15 mol) of methanesulfonyl chloride and 25.8 ml (0.19 mol) of triethylamine were added at 0° C. and stirred at room temperature for 1 hour. The reaction mixture was diluted with methylene chloride (100 ml) and successively washing with water (100 ml) and saturated saline (100 ml), followed by drying over anhydrous sodium sulfate. The solvent was then distilled off under vacuum to obtain 24.5 g (quant.) of the above-identified compound as a slightly brown crystal.

후처리

  1. washsuccessively washing with water (100 ml) and saturated saline (100 ml)
  2. dry with materialby drying over anhydrous sodium sulfate
  3. distillationThe solvent was then distilled off under vacuum
  4. customto obtain 24.5 g (quant.) of the above-identified compound as a slightly brown crystal

출처 및 근거

ORD 기록
ord-9332a5eff53840b7b73ba6a6f266a355
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06331548B1

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