反応式
B(Br)(Br)Br.ClCCl.[CH:8]1([CH2:11][N:12]([CH2:34][CH:35]2[CH2:37][CH2:36]2)[C:13]2[C:14]([S:32][CH3:33])=[N:15][N:16]3[C:21]([C:22]4[C:27]([CH3:28])=[CH:26][C:25]([CH3:29])=[CH:24][C:23]=4[O:30]C)=[CH:20][CH:19]=[CH:18][C:17]=23)[CH2:10][CH2:9]1.C(OCC)(=O)C>ClCCl>[CH:8]1([CH2:11][N:12]([CH2:34][CH:35]2[CH2:37][CH2:36]2)[C:13]2[C:14]([S:32][CH3:33])=[N:15][N:16]3[C:21]([C:22]4[C:27]([CH3:28])=[CH:26][C:25]([CH3:29])=[CH:24][C:23]=4[OH:30])=[CH:20][CH:19]=[CH:18][C:17]=23)[CH2:9][CH2:10]1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
A 1 M boron tribromide/dichloromethane solution (0.42 mL) was added to a solution of N,N-dicyclopropylmethyl-N-[7-(2-methoxy-4,6-dimethylphenyl)-2-(methylsulfanyl)pyrazolo[1,5-a]pyridin-3-yl]amine (35 mg) in dichloromethane (10 mL) at room temperature under a nitrogen atmosphere, and the mixture was stirred for 10 minutes. The reaction mixture was added to ice water, extraction was performed with ethyl acetate, and the organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained residue was subjected to silica gel column chromatography, and the title compound (17 mg) was obtained from the n-hexane:ethyl acetate (6:1) fraction as white crystals.
後処理
- washthe organic layer was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-7700df5685184235ac02c3c0c47a1faa
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07091215B2
関連ノート
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