Chloroacetonitrile → (Pyridine-3-sulphonyl)-acetonitrile

HRID 636425노트

반응식

HRID 636425 반응식
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

참가 물질

4

반응물 2

HCID 7856ChloroacetonitrileHCID 23697071Sodium pyridine-3-sulfinate

생성물 1

HCID 21254898(Pyridine-3-sulphonyl)-acetonitrile수율 80%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-71acbc7dcf784c80b3ea50e3335f3874
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194410B1

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