Acetone → 7-Methoxy-1-(2-pyridyl)-3,6,6-trimethyl-4-oxo-4,5,6,7-tetrahydroindazole

HRID 2084283

반응식

HRID 2084283 반응식
Br[CH:2]1[C:10]2[N:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=3)[N:8]=[C:7]([CH3:17])[C:6]=2[C:5](=[O:18])[CH2:4][C:3]1([CH3:20])[CH3:19].C[C:22](C)=[O:23]>CO.[N+]([O-])([O-])=O.[Ag+]>[CH3:22][O:23][CH:2]1[C:10]2[N:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=3)[N:8]=[C:7]([CH3:17])[C:6]=2[C:5](=[O:18])[CH2:4][C:3]1([CH3:20])[CH3:19]

참가 물질

5

반응물 2

HCID 180AcetoneHCID 40739867-Bromo-3,6,6-trimethyl-1-pyridin-2-yl-5,7-dihydroindazol-4-one

생성물 1

HCID 98606407-Methoxy-1-(2-pyridyl)-3,6,6-trimethyl-4-oxo-4,5,6,7-tetrahydroindazole수율 25%

시약·촉매·용매 2

HCID 24470Silver Nitrate촉매2회HCID 887Methanol용매2회

실험 절차

A solution of 0.1N silver nitrate in methanol (12 ml, 1.2 mmol) was added to a solution of 7-bromo-1-(2-pyridyl)-3,6,6-trimethyl-4-oxo-4,5,6,7-tetrahydroindazole (0.2 g, 0.6 mmol), prepared as described in example 4, in acetone (12 ml). After stirring for about 48 hours, 6 ml of a 0.1N silver nitrate solution in methanol were added. The reaction mixture was stirred for further 72 hours and then filtered. The solvent was evaporated and the residue was chromatographed on silica gel (cyclohexane:ethyl acetate=90:10) to yield the title compound as a colourless solid (0.044 g, 25%): m.p. 86-89° C.

후처리

  1. customprepared
  2. stirringThe reaction mixture was stirred for further 72 hours
  3. filtrationfiltered
  4. customThe solvent was evaporated
  5. customthe residue was chromatographed on silica gel (cyclohexane:ethyl acetate=90:10)

출처 및 근거

ORD 기록
ord-b396a51757a74b9086b66f18d74683dc
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06716856B1

연결된 노트

불러오는 중…