反応式
[C:1]([C@H:5]1[C@@H:11]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH2:10][C@H:9]2[N:19]([CH3:20])[C@@H:6]1[CH2:7][CH2:8]2)([O:3]C)=[O:2]>O1CCOCC1.O>[C:1]([C@H:5]1[C@@H:11]([C:12]2[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=2)[CH2:10][C@H:9]2[N:19]([CH3:20])[C@@H:6]1[CH2:7][CH2:8]2)([OH:3])=[O:2]参加物
3
実験手順
2β-Carbomethoxy-3β-(4-fluorophenyl)tropane (WIN 35,428) (1), is boiled for 24 h in a 1:1 dioxane-water solution. The solvent is removed in vacuo and the residue is almost completely dissolved in CHCl3. Remaining undissolved solid can then be filtered off, toluene can then be added, and the volume of the solution is reduced in vacuo to approximately 25%. Cooling the resulting white suspension in a freezer for 2 h will provide a precipitated solid which can then be isolated by filtration and is washed with cold 1:1 CHCl3-toluene. The solid can then be pumped dry to give the product.
後処理
- customThe solvent is removed in vacuo
- dissolutionthe residue is almost completely dissolved in CHCl3
- filtrationcan then be filtered off
- additiontoluene can then be added
- temperatureCooling the resulting white suspension in a freezer for 2 h
- customwill provide a precipitated solid which
- customcan then be isolated by filtration
- washis washed with cold 1:1 CHCl3-toluene
- customThe solid can then be pumped dry
- customto give the product
出典と根拠
- ORDレコード
- ord-3550ea0a7d1f4d248e4c52837af96eb5
- 出典データセット
- uspto-grants-2009_01
- 特許番号
- US07476740B2
関連ノート
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