反応式
[F:1][C:2]1[CH:20]=[CH:19][C:5]2[C:6]([CH2:9][CH2:10][CH2:11][N:12]3[CH2:17][CH2:16][C:15](=[O:18])[CH2:14][CH2:13]3)=[N:7][O:8][C:4]=2[CH:3]=1.C([Mg]Br)[C:22]1[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[CH:24][CH:23]=1.[Cl-:32].[NH4+]>O1CCCC1.CCOCC>[ClH:32].[F:1][C:2]1[CH:20]=[CH:19][C:5]2[C:6]([CH2:9][CH2:10][CH2:11][N:12]3[CH2:13][CH2:14][C:15]([OH:18])([C:22]4[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[CH:24][CH:23]=4)[CH2:16][CH2:17]3)=[N:7][O:8][C:4]=2[CH:3]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 2
実験手順
A solution of 6.3 g of 1-[3-(6-fluoro-1,2-benzisoxazol-3-yl)propyl]-4-piperidone in 35 ml of tetrahydrofuran was slowly added to a solution of 49 ml of p-anisylmagnesium bromide (1.4 M in tetrahydrofuran). After the addition was complete, the reaction mixture was stirred at ambient temperature for one hr, diluted with ether, poured into 400 of ml saturated ammonium chloride solution and extracted with ether. The organic extracts were washed with water (2×), saturated sodium chloride solution and dried over anhydrous magnesium sulfate, filtered and concentrated. The residue was converted to 8.5 g (89%) of product, mp 100°-105° C., by treatment with ethereal hydrogen chloride. An analytical sample was obtained by recrystallization from ethyl acetate/methanol and had mp 181°-182° C. (dec).
後処理
- additionAfter the addition
- extractionextracted with ether
- washThe organic extracts were washed with water (2×), saturated sodium chloride solution
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customAn analytical sample was obtained by recrystallization from ethyl acetate/methanol
出典と根拠
- ORDレコード
- ord-c19ce0116b8849bba4849a32a844be42
- 出典データセット
- uspto-grants-1983_08
- 特許番号
- US04396770
関連ノート
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