Triethylamine → Oxetan-3-ylmethyl methanesulfonate

HRID 1915873노트

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HRID 1915873 반응식
[O:1]1[CH2:4][CH:3]([CH2:5][OH:6])[CH2:2]1.C(N(CC)CC)C.[CH3:14][S:15](Cl)(=[O:17])=[O:16]>C(Cl)Cl>[CH3:14][S:15]([O:6][CH2:5][CH:3]1[CH2:4][O:1][CH2:2]1)(=[O:17])=[O:16]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 11521066Oxetan-3-ylmethanol

생성물 1

HCID 86680078Oxetan-3-ylmethyl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

Oxetan-3-ylmethanol (1.85 g, 21.0 mmol) was dissolved in methylene chloride and cooled to 0° C. Triethylamine (5.31 g, 52.2 mmol) was added followed by slow addition of methanesulfonyl chloride (2.89 g, 25.2 mmol). The mixture was allowed to warm to ambient temperature for 2 h and quenched with sat. sodium bicarbonate (14 mL). The aqueous solution was extracted with methylene chloride 3×. The combined organic layers were dried over sodium sulfate, filtered and concentrated to give crude oxetan-3-ylmethyl methanesulfonate (quant.).

후처리

  1. temperatureto warm to ambient temperature for 2 h
  2. customquenched with sat. sodium bicarbonate (14 mL)
  3. extractionThe aqueous solution was extracted with methylene chloride 3×
  4. dry with materialThe combined organic layers were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3452a4ced46a404d9ad0478512be16b4
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614206B2

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