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

HRID 916849ノート

反応式

HRID 916849 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3eea76d6a04b421aa5dbf77cba9a1981
出典データセット
uspto-grants-2007_09
特許番号
US07271197B2

反応ノート

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