反応式
[ClH:1].Cl.[F:3][C:4]([F:25])([F:24])[C:5]1[CH:10]=[CH:9][C:8]([C:11]2[N:16]=[N:15][C:14]([N:17]3[CH2:23][CH2:22][CH2:21][NH:20][CH2:19][CH2:18]3)=[CH:13][CH:12]=2)=[CH:7][CH:6]=1.C(N(CC)CC)C.[H-].[Na+].[Cl:35][CH:36]([CH3:38])[CH3:37]>C1COCC1.CN(C)C=O>[ClH:35].[ClH:1].[CH:36]([N:20]1[CH2:21][CH2:22][CH2:23][N:17]([C:14]2[N:15]=[N:16][C:11]([C:8]3[CH:9]=[CH:10][C:5]([C:4]([F:24])([F:3])[F:25])=[CH:6][CH:7]=3)=[CH:12][CH:13]=2)[CH2:18][CH2:19]1)([CH3:38])[CH3:37]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
4-[6-(4-Trifluoromethylphenyl)pyridazin-3-yl][1,4]diazepane, dihydrochloride (0.028 g, 0.071 mmol) was suspended in THF (4 mL) and triethylamine (0.022 g, 0.21 mmol) was added. Sodium hydride (0.0085 g, 0.35 mmol) was added and the reaction mixture was stirred at rt for 20 min. Dry N,N-dimethylformamide (1 mL) and 2-chloropropane (0.056 g, 0.71 mmol) was added and the reaction mixture was heated 30 min at 160° C. and 30 min at 180° C. in a microwave oven. The reaction mixture was purified on a silicagel column (0.04-0.063 mesh) using dichloromethane/MeOH (9:1) as eluent. This afforded a crude oil containing several components that was purified further by preparative HPLC using Method B. This afforded 9 mg of an oil which was dissolved into MeOH. Addition of HCl in diethyl ether afforded 6.5 mg (21%) of the title compound as an oily dihydrochloride.
後処理
- temperaturethe reaction mixture was heated 30 min at 160° C. and 30 min at 180° C. in a microwave oven
- customThe reaction mixture was purified on a silicagel column (0.04-0.063 mesh)
- customThis afforded a crude oil
- additioncontaining several components that
- customwas purified further by preparative HPLC
- dissolutionThis afforded 9 mg of an oil which was dissolved into MeOH
- additionAddition of HCl in diethyl ether
出典と根拠
- ORDレコード
- ord-48faf4b9d2b044d9ba597e68eb6d8c3d
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846677B2
関連ノート
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