Chloroacetonitrile → HCID 21823271、化合物

HRID 636423ノート

反応式

HRID 636423 の反応式
Cl[CH2:2][C:3]#[N:4].[Na+].[C:6]1([CH3:15])[CH:11]=[CH:10][CH:9]=[C:8]([S:12]([O-:14])=[O:13])[CH:7]=1>CN(C=O)C>[C:6]1([CH3:15])[CH:11]=[CH:10][CH:9]=[C:8]([S:12]([CH2:2][C:3]#[N:4])(=[O:14])=[O:13])[CH:7]=1

参加物

4

反応物 2

HCID 7856ChloroacetonitrileHCID 23703014Sodium 3-methylbenzene-1-sulfinate

生成物 1

HCID 21823271HCID 21823271、化合物収率 25.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2.65 ml (42 mmol) of chloroacetonitrile were added to a suspension of 7.5 g (42 mmol) of toluene-3-sulphinic acid sodium salt in 80 ml of DMF and stirred at 100° for 1 hr. The reaction solution was evaporated, the residue was partitioned between H2O and CH2Cl2. The aqueous phase was washed three times with CH2Cl2. The combined organic phases were washed once with H2O, dried (MgSO4). filtered and evaporated. Chromatography (SiO2, CH2Cl2) yielded 2.06 g (25%) of (toluene-3-sulphonyl)-acetonitrile as a colorless oil.

後処理

  1. customThe reaction solution was evaporated
  2. customthe residue was partitioned between H2O and CH2Cl2
  3. washThe aqueous phase was washed three times with CH2Cl2
  4. washThe combined organic phases were washed once with H2O
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-3c2d35598e2b4f1d88e1d600ef85c5df
出典データセット
uspto-grants-2001_02
特許番号
US06194410B1

反応ノート

読み込み中…