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

HRID 2389339ノート

反応式

HRID 2389339 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-a9321fd5737c4d248f7349700d35d2ba
出典データセット
uspto-grants-2012_09
特許番号
US08273745B2

反応ノート

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