Chloroacetonitrile → (Pyridine-3-sulphonyl)-acetonitrile

HRID 636425ノート

反応式

HRID 636425 の反応式
Cl[CH2:2][C:3]#[N:4].[Na+].[N:6]1[CH:11]=[CH:10][CH:9]=[C:8]([S:12]([O-:14])=[O:13])[CH:7]=1>CN(C=O)C>[N:6]1[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 23697071Sodium pyridine-3-sulfinate

生成物 1

HCID 21254898(Pyridine-3-sulphonyl)-acetonitrile収率 80%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2.1 ml (33.4 mmol) of chloroacetonitrile were added to a solution of 4.6 g (42 mmol) of pyridine-3-sulphinic acid sodium salt in 50 ml of DMF and stirred at 90° 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, AcOEt/hexane 2:1) yielded 4.1 g (80%) of (pyridine-3-sulphonyl)-acetonitrile as a beige solid.

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-71acbc7dcf784c80b3ea50e3335f3874
出典データセット
uspto-grants-2001_02
特許番号
US06194410B1

反応ノート

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