2,3-Butanediol → 2,3-Butanediol, dimethanesulfonate

HRID 85381

반응식

HRID 85381 반응식
[CH3:1][CH:2]([OH:6])[CH:3]([OH:5])[CH3:4].CCN(CC)CC.[CH3:14][S:15](Cl)(=[O:17])=[O:16]>C(Cl)Cl>[CH3:14][S:15]([O:5][CH:3]([CH:2]([O:6][S:15]([CH3:14])(=[O:17])=[O:16])[CH3:1])[CH3:4])(=[O:17])=[O:16]

참가 물질

5

반응물 3

HCID 2622,3-ButanediolHCID 8471TriethylamineHCID 31297Methanesulfonyl chloride

생성물 1

HCID 999092,3-Butanediol, dimethanesulfonate수율 98%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

반응 조건

온도
0 °C

실험 절차

To a solution of butane 2,3-diol (15 g, 0.166 mol) and Et3N (57.7 mL, 0.415 mol) in CH2Cl2 (150 mL) at 0° C. was slowly added a solution of CH3SO2Cl (32.1 mL, 0.415 mol) in CH2Cl2 (75 mL). The mixture was stirred at 0° C. for 2 h and diluted with CH2Cl2. The mixture was washed with water, 1N HCl, 5% aqueous NaHCO3 and brine. The organic layer was dried over MgSO4, filtered and concentrated under reduced pressure to afford butane-2,3-diol dimethanesulfonate (40 g, 98%) as a light yellow oil. 1HNMR (CDCl3): δ 4.9 (m, 2H, CH), 3.05 (s, 6H, CH3), 1.4 (m, 6H, CH3).

후처리

  1. washThe mixture was washed with water, 1N HCl, 5% aqueous NaHCO3 and brine
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0f3fd8bb40ac42499f2ea47afda727b8
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846972B2

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