Benzyl Bromide → 3-Benzyloxy-2-iodopyridine

HRID 55257

반응식

HRID 55257 반응식
C(=O)([O-])[O-].[K+].[K+].[OH:7][C:8]1[C:9]([I:14])=[N:10][CH:11]=[CH:12][CH:13]=1.[CH2:15](Br)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>CN(C)C=O.C(=O)([O-])[O-].[Cs+].[Cs+]>[CH2:15]([O:7][C:8]1[C:9]([I:14])=[N:10][CH:11]=[CH:12][CH:13]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

6

반응물 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 971792-Iodopyridin-3-ol

생성물 1

HCID 199575013-Benzyloxy-2-iodopyridine

시약·촉매·용매 2

HCID 10796Cesium carbonate촉매HCID 6228Dimethylformamide용매

실험 절차

152.6 g of potassium carbonate and 15.3 g of cesium carbonate are added to a solution of 122 g of 3-hydroxy-2-iodopyridine and 65.7 ml of benzyl bromide in 1.5 l of dimethylformamide, and the suspension is stirred under argon atmosphere for 20 hours at room temperature. The reaction mixture is filtered, the filter residue is washed with dichloromethane, the filtrate is concentrated by evaporation, and the residue is chromatographed on silica gel with hexane/10-20% ethyl acetate. 146.3 g of 3-benzyloxy-2-iodopyridine is obtained as oil.

후처리

  1. filtrationThe reaction mixture is filtered
  2. washthe filter residue is washed with dichloromethane
  3. concentrationthe filtrate is concentrated by evaporation
  4. customthe residue is chromatographed on silica gel with hexane/10-20% ethyl acetate

출처 및 근거

ORD 기록
ord-e2e957f3b549479c94a5f8e24c545d13
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624943

연결된 노트

불러오는 중…