Potassium thiocyanate → HCID 10655699、化合物

HRID 274286ノート

反応式

HRID 274286 の反応式
Cl[CH2:2][CH2:3][C:4]([CH3:11])([CH3:10])[C:5]([O:7][CH2:8][CH3:9])=[O:6].[S-:12][C:13]#[N:14].[K+]>CN(C)C=O.O>[CH3:10][C:4]([CH3:11])([CH2:3][CH2:2][S:12][C:13]#[N:14])[C:5]([O:7][CH2:8][CH3:9])=[O:6]

参加物

5

反応物 2

HCID 516872Potassium thiocyanateHCID 10797430Ethyl 4-chloro-2,2-dimethylbutanoate

生成物 1

HCID 10655699HCID 10655699、化合物収率 65.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

In 100 ml of dimethylformamide were dissolved 22.1 g of ethyl 4-chloro-2,2-dimethylbutyrate and 14.5 g of potassium thiocyanate and the solution was stirred at 100° C. for 7 hours. The reaction mixture was poured in 500 ml of water and extracted with ethyl ether. The extract was washed with water and dried (MgSO4) and the solvent was distilled off. The residue was subjected to vacuum distillation to provide 16.4 g of the title compound as colorless oil. b.p. 109°-111° C./0.3 mmHg

後処理

  1. extractionextracted with ethyl ether
  2. washThe extract was washed with water
  3. dry with materialdried (MgSO4)
  4. distillationthe solvent was distilled off
  5. distillationThe residue was subjected to vacuum distillation

出典と根拠

ORDレコード
ord-523cc06023b34faaad3d5774d551a396
出典データセット
uspto-grants-1995_02
特許番号
US05389633

反応ノート

読み込み中…