反応式
[CH3:1][C@@:2]12[C@@H:10]([C:11]([NH:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:9][CH2:8][C@H:7]1[C@@H:6]1[CH2:18][CH2:19][C@H:20]3[NH:26][C:24](=[O:25])[CH:23]=[CH:22][C@:21]3([CH3:27])[C@H:5]1[CH2:4][CH2:3]2.[Br-:28].[Li+:29]>C(Cl)Cl>[CH3:1][C@@:2]12[C@@H:10]([C:11]([NH:13][C:14]([CH3:15])([CH3:16])[CH3:17])=[O:12])[CH2:9][CH2:8][C@H:7]1[C@@H:6]1[CH2:18][CH2:19][C@H:20]3[NH:26][C:24](=[O:25])[CH:23]=[CH:22][C@:21]3([CH3:27])[C@H:5]1[CH2:4][CH2:3]2.[Br-:28].[Li+:29]参加物
実験手順
Into a 100 ml r.b. flask equipped with a magnetic stirrer and a nitrogen inert atmosphere was weighted 3.71 gm of finasteride. Methylene chloride (20 ml) was added and the slurry astirred to dissolve the substrate. To the clear light yellow solution was added 0.87 g of anhydrous lithium bromide. The solid was washed down into the reaction with 5 ml of methylene chloride. The slurry was stirred. Within one minute add 1 drop of n-propanol from a disposable pipette. The slurry was stirred overnight with exclusion of moisture under an inert nitrogen atmosphere. The slurry is filtered on a Buchner funnel and the flask and solid washed with 10 ml of methylene chloride. After drying the solid at 50° C. in vacuum the solid complex weighs 4.17 g. The methylene chloride solution contains 0.35 g of nonvolatile residue.
後処理
- customflask equipped with a magnetic stirrer
- dissolutionto dissolve the substrate
- washThe solid was washed down into the reaction with 5 ml of methylene chloride
- additionWithin one minute add 1 drop of n-propanol from a disposable pipette
- stirringThe slurry was stirred overnight with exclusion of moisture under an inert nitrogen atmosphere
- filtrationThe slurry is filtered on a Buchner funnel
- washthe flask and solid washed with 10 ml of methylene chloride
- customAfter drying the solid at 50° C. in vacuum the solid complex
出典と根拠
- ORDレコード
- ord-72e4a8d9898d44bb934a528578204d0f
- 出典データセット
- uspto-grants-2004_01
- 特許番号
- US06677453B1
関連ノート
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