Water → Ethyl (3-{3-[(methylsulfonyl)oxy]propyl}phenoxy)acetate

HRID 2389339노트

반응식

HRID 2389339 반응식
[OH:1][CH2:2][CH2:3][CH2:4][C:5]1[CH:6]=[C:7]([CH:15]=[CH:16][CH:17]=1)[O:8][CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11].[CH3:18][S:19](Cl)(=[O:21])=[O:20].O>C(Cl)Cl>[CH3:18][S:19]([O:1][CH2:2][CH2:3][CH2:4][C:5]1[CH:6]=[C:7]([CH:15]=[CH:16][CH:17]=1)[O:8][CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])(=[O:21])=[O:20]

참가 물질

5

반응물 3

HCID 962WaterHCID 31297Methanesulfonyl chlorideHCID 86637895Ethyl [3-(3-hydroxypropyl)phenoxy]acetate

생성물 1

HCID 86637907Ethyl (3-{3-[(methylsulfonyl)oxy]propyl}phenoxy)acetate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of ethyl [3-(3-hydroxypropyl)phenoxy]acetate (107.4 g) in DCM (1.07 L) was added TEA (113 mL) at ambient temperature. Methanesulfonyl chloride (45.4 mL) was added dropwise to the mixture at 0° C. The mixture was stirred for 1 hour at ambient temperature and water (1 L) was added to the mixture at the same temperature. The organic layer was washed with brine, dried over anhydrous MgSO4, filtered and evaporated in vacuo to afford ethyl (3-{3-[(methylsulfonyl)oxy]propyl}phenoxy)acetate (155.5 g) as a yellow oil.

후처리

  1. washThe organic layer was washed with brine
  2. dry with materialdried over anhydrous MgSO4
  3. filtrationfiltered
  4. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-a9321fd5737c4d248f7349700d35d2ba
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08273745B2

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