Tin dichloride dihydrate → 6-Cyclopropyl-5-phenylpyridin-3-amine

HRID 41990

반응식

HRID 41990 반응식
[CH:1]1([C:4]2[C:9]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)=[CH:8][C:7]([N+:16]([O-])=O)=[CH:6][N:5]=2)[CH2:3][CH2:2]1.Cl[Sn]Cl.O>C(O)C>[CH:1]1([C:4]2[N:5]=[CH:6][C:7]([NH2:16])=[CH:8][C:9]=2[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 43835034Tin dichloride dihydrateHCID 673947372-Cyclopropyl-5-nitro-3-phenylpyridine

생성물 1

HCID 584158326-Cyclopropyl-5-phenylpyridin-3-amine수율 57.1%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

A mixture of 2-cyclopropyl-5-nitro-3-phenylpyridine (0.25 mmol, 0.06 g) and SnCl2.H2O (0.89 mmol, 0.2 g) in ethanol (2 ml) was heated at 80° C. for 1 hour. The solvent was evaporated and the crude residue was dissolved in water. The solution neutralised with 6N NaOH aqueous solution and extracted with dichloromethane. The solid residue was purified by chromatography over SiO2 eluting with dichloromethane/methanol mixtures affording 6-cyclopropyl-5-phenylpyridin-3-amine (0.03 g, 57% of yield) of the expected product.

후처리

  1. customThe solvent was evaporated
  2. dissolutionthe crude residue was dissolved in water
  3. extractionextracted with dichloromethane
  4. customThe solid residue was purified by chromatography over SiO2 eluting with dichloromethane/methanol

출처 및 근거

ORD 기록
ord-e2d2246eb6a34499a6fbd94959555ffd
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536165B2

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