Dimethylformamide → 2-(6-Chlorobenzo[d][1,3]dioxol-5-yl)acetonitrile

HRID 1586279

反応式

HRID 1586279 の反応式
[CH2:1]1[O:5][C:4]2[CH:6]=[C:7]([Cl:12])[C:8]([CH2:10]Cl)=[CH:9][C:3]=2[O:2]1.[CH3:13][N:14](C)C=O.[C-]#N.[K+]>O>[Cl:12][C:7]1[C:8]([CH2:10][C:13]#[N:14])=[CH:9][C:3]2[O:2][CH2:1][O:5][C:4]=2[CH:6]=1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 9032Potassium CyanideHCID 901136-Chloropiperonyl chloride

生成物 1

HCID 212181222-(6-Chlorobenzo[d][1,3]dioxol-5-yl)acetonitrile

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1.025 g of 6-chloropiperonyl chloride, 5 ml of dimethylformamide, 330 mg of potassium cyanide are introduced, agitation is carried out at ambient temperature for 6 hours, the reaction medium is poured into 50 ml of water, extracted with 3×30 ml of ethyl acetate, the extracts are washed with 30 ml of sodium chloride and dried. After recrystallization from 5 ml of isopropyl ether under reflux and separating, 740 mg of expected product (white crystals) is obtained. ANALYSIS: IR CHCl3 cm-1CN 2255 Aromatic 1625-1505-1481

後処理

  1. extractionextracted with 3×30 ml of ethyl acetate
  2. washthe extracts are washed with 30 ml of sodium chloride
  3. customdried
  4. customAfter recrystallization from 5 ml of isopropyl ether
  5. temperatureunder reflux
  6. customseparating

出典と根拠

ORDレコード
ord-83afbb4c0fb64d549bba377b9ba0c0c3
出典データセット
uspto-grants-1999_08
特許番号
US05942622

関連ノート

読み込み中…