N-(1-propenyl)piperidine → 1-(4-Fluorophenyl)-4-methyl-5-piperidino-4,5-dihydro-1,2,3-triazole
反応式
[CH:1]([N:4]1[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1)=[CH:2][CH3:3].[F:10][C:11]1[CH:16]=[CH:15][C:14]([N:17]=[N+:18]=[N-:19])=[CH:13][CH:12]=1>>[F:10][C:11]1[CH:16]=[CH:15][C:14]([N:17]2[CH:1]([N:4]3[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]3)[CH:2]([CH3:3])[N:19]=[N:18]2)=[CH:13][CH:12]=1参加物
3
実験手順
1-(1-propenyl)-piperidine (9.4 g; 75.07 mmol) and 4-fluorophenylazide (10.3 g; 75.07 mmol), prepared as described in example 1, were admixed at 0° C. and the resultant mixture was kept at room temperature for 54 hours in the absence of light. The obtained solid mass was collected with petroleum ether and filtered obtaining the title compound (6 g). The mother liquor was evaporated and the resultant crude compound was purified by chromatography on silica gel (230-400 mesh), eluent petroleum ether:ethyl acetate=9:1, obtaining further title compound (m.p. 75° 76° C.).
後処理
- customwere admixed at 0° C.
- customThe obtained solid mass was collected with petroleum ether
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-62ca70e0b3a2422f8caaa317d2c841fc
- 出典データセット
- uspto-grants-1992_01
- 特許番号
- US05081136
反応ノート
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