Pyridine → 2-(3-(Chloromethyl)-5-(2-cyanopropan-2-yl)phenyl)-2-methylpropanenitrile

HRID 1636803ノート

反応式

HRID 1636803 の反応式
O[CH2:2][C:3]1[CH:4]=[C:5]([C:14]([CH3:18])([CH3:17])[C:15]#[N:16])[CH:6]=[C:7]([C:9]([CH3:13])([CH3:12])[C:10]#[N:11])[CH:8]=1.N1C=CC=CC=1.S(Cl)([Cl:27])=O>ClCCl>[Cl:27][CH2:2][C:3]1[CH:4]=[C:5]([C:14]([CH3:18])([CH3:17])[C:15]#[N:16])[CH:6]=[C:7]([C:9]([CH3:13])([CH3:12])[C:10]#[N:11])[CH:8]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 193493981,3-Benzenediacetonitrile, 5-(hydroxymethyl)-alpha1,alpha1,alpha3,alpha3-tetramethyl-

生成物 1

HCID 193493842-(3-(Chloromethyl)-5-(2-cyanopropan-2-yl)phenyl)-2-methylpropanenitrile

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 2,2'-(5-hydroxymethyl-1,3-phenylene)di-(2-methylpropiononitrile), (3.8 g) and pyridine (1.58 g) in dichloromethane (10 ml) was stirred, and cooled in an ice bath, while thionyl chloride (3 g) was added over 10 minutes. The solution was kept at room temperature for 2 h and then heated under reflux for 1 h and evaporated to dryness under reduced pressure The residue was partitioned between water and ethyl acetate and the organic phase was separated, dried and evaporated to dryness under reduced pressure to give 2,2'-(5-chloromethyl-1,3-phenylene)di(2-methylpropiononitrile), which was used without further purification.

後処理

  1. additionwas added over 10 minutes
  2. temperatureheated
  3. temperatureunder reflux for 1 h
  4. customevaporated to dryness under reduced pressure The residue
  5. customwas partitioned between water and ethyl acetate
  6. customthe organic phase was separated
  7. customdried
  8. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-59bbcfffe7ec4d61b604b6bb29415ee1
出典データセット
uspto-grants-2000_03
特許番号
USRE036617

反応ノート

読み込み中…