Triethylamine → 3-(Diethoxymethyl)phenethyl methanesulfonate

HRID 471011노트

반응식

HRID 471011 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH2:6]([O:8][CH:9]([O:19][CH2:20][CH3:21])[C:10]1[CH:11]=[C:12]([CH2:16][CH2:17][OH:18])[CH:13]=[CH:14][CH:15]=1)[CH3:7].C(N(CC)CC)C>ClCCl>[CH3:1][S:2]([O:18][CH2:17][CH2:16][C:12]1[CH:13]=[CH:14][CH:15]=[C:10]([CH:9]([O:8][CH2:6][CH3:7])[O:19][CH2:20][CH3:21])[CH:11]=1)(=[O:4])=[O:3]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 579893032-(3-(Diethoxymethyl)phenyl)ethanol

생성물 1

HCID 579889463-(Diethoxymethyl)phenethyl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Methanesulfonyl chloride (0.18 g) in dichloromethane (0.2 mL) was added to a stirred solution of 2-(3-(diethoxymethyl)phenyl)ethanol (example 20, step c) (0.23 g) and triethylamine (0.429 mL) in dichloromethane (2.5 mL) cooled in an ice bath. After 1 h, the reaction mixture was partitioned between ethyl acetate and saturated sodium bicarbonate solution. The ethyl acetate layer was washed with saturated sodium bicarbonate solution and brine, dried over sodium sulphate, filtered and evaporated in vacuo to give the subtitled compound as a gum. Yield 0.28 g.

후처리

  1. temperaturecooled in an ice bath
  2. customthe reaction mixture was partitioned between ethyl acetate and saturated sodium bicarbonate solution
  3. washThe ethyl acetate layer was washed with saturated sodium bicarbonate solution and brine
  4. dry with materialdried over sodium sulphate
  5. filtrationfiltered
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-89a08a0dc47e45da9cc190d2975334d5
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629271B2

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