Methanesulfonyl chloride → 2-[(3-Cyanobenzyl)oxy]ethyl methanesulfonate

HRID 916849노트

반응식

HRID 916849 반응식
[OH:1][CH2:2][CH2:3][O:4][CH2:5][C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][CH:13]=1)[C:9]#[N:10].C(N(C(C)C)CC)(C)C.[CH3:23][S:24](Cl)(=[O:26])=[O:25]>ClCCl>[CH3:23][S:24]([O:1][CH2:2][CH2:3][O:4][CH2:5][C:6]1[CH:13]=[CH:12][CH:11]=[C:8]([C:9]#[N:10])[CH:7]=1)(=[O:26])=[O:25]

참가 물질

5

반응물 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 284140323-[(2-Hydroxyethoxy)methyl]benzonitrile

생성물 1

HCID 858813992-[(3-Cyanobenzyl)oxy]ethyl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-[(2-hydroxyethoxy)methyl]benzonitrile (example 28vi) (6.00 g) and diisopropylethylamine (11.8 ml) in dichloromethane (100 ml) at 0° C. was added methanesulphonyl chloride (3.14 ml) dropwise and the mixture allowed to stir for 2 h. The resultant mixture was partitioned between dichloromethane and saturated sodium hydrogen carbonate. The organic phase was dried (MgSO4) and concentrated in vacuo to give the title compound (8.5 g). LCMS RT=2.58 min.

후처리

  1. customat 0° C.
  2. customThe resultant mixture was partitioned between dichloromethane and saturated sodium hydrogen carbonate
  3. dry with materialThe organic phase was dried (MgSO4)
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3eea76d6a04b421aa5dbf77cba9a1981
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07271197B2

반응 노트

불러오는 중…