Water → Methanesulfonic acid 2-(4-chloro-benzyloxy)-ethyl ester

HRID 2261245노트

반응식

HRID 2261245 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[Cl:6][C:7]1[CH:17]=[CH:16][C:10]([CH2:11][O:12][CH2:13][CH2:14][OH:15])=[CH:9][CH:8]=1.C(N(C(C)C)CC)(C)C.O>C(Cl)Cl>[Cl:6][C:7]1[CH:8]=[CH:9][C:10]([CH2:11][O:12][CH2:13][CH2:14][O:15][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:16][CH:17]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 27637512-[(4-Chlorobenzyl)oxy]-1-ethanol

생성물 1

HCID 59593471Methanesulfonic acid 2-(4-chloro-benzyloxy)-ethyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of methanesulfonyl chloride (980 μL, 12.6 mmol) in dry DCM (10 mL) was slowly added to a cooled (0° C.) solution of 2-(4-chloro-benzyloxy)-ethanol (2.14 g, 11.46 mmol) and diisopropyethylamine (2.0 mL, 23 mmol) in dry DCM (10 mL). The reaction mixture was allowed to warm to RT overnight. Water was added and the organic layer was dried (MgSO4) and concentrated. The residue was purified by column chromatography over silica using a gradient of 0-20% diethyl ether/cyclohexane to afford the pure product.

후처리

  1. dry with materialthe organic layer was dried (MgSO4)
  2. concentrationconcentrated
  3. customThe residue was purified by column chromatography over silica using a gradient of 0-20% diethyl ether/cyclohexane
  4. customto afford the pure product

출처 및 근거

ORD 기록
ord-58bc85cb922144c3bfaba53750531d1d
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07846955B2

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