Water → 2-(2-Chloroethoxy)ethyl methanesulfonate

HRID 2226763

반응식

HRID 2226763 반응식
[Cl:1][CH2:2][CH2:3][O:4][CH2:5][CH2:6][OH:7].C(N(CC)CC)C.[CH3:15][S:16](Cl)(=[O:18])=[O:17].O>C1(C)C=CC=CC=1>[S:16]([O:7][CH2:6][CH2:5][O:4][CH2:3][CH2:2][Cl:1])(=[O:18])(=[O:17])[CH3:15]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 123612-(Chloroethoxy)ethanolHCID 31297Methanesulfonyl chloride

생성물 1

HCID 212173742-(2-Chloroethoxy)ethyl methanesulfonate

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
5 °C

실험 절차

To a solution of 2-(2-chloroethoxy)ethanol (15.3 g, 123 mmol) in toluene (100 ml) kept at 5° C. was added triethylamine (50 g, 500 mmol). A solution of methanesulfonyl chloride (28 g, 245 mmol) in toluene (50 ml) was carefully added keeping the temperature around 5° C. When addition was complete the reaction mixture was stirred at 5° C. for 45 minutes and then 75 minutes at ambient temperature. Water (100 ml) was added and the mixture was stirred for 15 minutes. The phases were separated and the organic phase was washed with water, brine and dried over magnesium sulphate. The solvent was evaporated in vacuo to give crude 2-(2-chloroethoxy)ethyl mesylate as an oil.

후처리

  1. customkept at 5° C.
  2. customthe temperature around 5° C
  3. additionWhen addition
  4. custom75 minutes
  5. customat ambient temperature
  6. stirringthe mixture was stirred for 15 minutes
  7. customThe phases were separated
  8. washthe organic phase was washed with water, brine
  9. dry with materialdried over magnesium sulphate
  10. customThe solvent was evaporated in vacuo

출처 및 근거

ORD 기록
ord-109ceabd173a4a51882d63eb6799949d
출처 데이터셋
uspto-grants-1994_09
특허 번호
US05348965

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