Solketal → (2,2-Dimethyl-1,3-dioxolan-4-yl)methyl methanesulfonate

HRID 79407노트

반응식

HRID 79407 반응식
[CH3:1][C:2]1([CH3:9])[O:6][CH:5]([CH2:7][OH:8])[CH2:4][O:3]1.[CH3:10][S:11](Cl)(=[O:13])=[O:12].C(N(CC)CC)C>C(Cl)Cl>[CH3:10][S:11]([O:8][CH2:7][CH:5]1[CH2:4][O:3][C:2]([CH3:9])([CH3:1])[O:6]1)(=[O:13])=[O:12]

참가 물질

5

반응물 3

HCID 7528SolketalHCID 8471TriethylamineHCID 31297Methanesulfonyl chloride

생성물 1

HCID 15570840(2,2-Dimethyl-1,3-dioxolan-4-yl)methyl methanesulfonate수율 100.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To (2,2-dimethyl-1,3-dioxolan-4-yl)methanol (400 mg, 3.03 mmol) in DCM (6 mL) at 0° C. was added methanesulfonyl chloride (381 mg, 3.33 mmol) and triethylamine (368 mg, 3.63 mmol. The cold bath was removed and the reaction mixture was stirred for 30 minutes. The mixture was diluted with DCM (5 mL). The organic phase was washed with water (4 mL) and brine (2 mL), and dried (Na2SO4). The solution was concentrated under reduced pressure to give the product (642 mg).

후처리

  1. customThe cold bath was removed
  2. additionThe mixture was diluted with DCM (5 mL)
  3. washThe organic phase was washed with water (4 mL) and brine (2 mL)
  4. dry with materialdried (Na2SO4)
  5. concentrationThe solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-c6973e2a5d534758b3d1c9b5b6305e53
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841455B2

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