反応式
[CH2:1]1[C:6]2[NH:7][C:8]3[C:13]([C:5]=2[CH2:4][C@H:3]([C:14]([OH:16])=[O:15])[NH:2]1)=[CH:12][CH:11]=[CH:10][CH:9]=3.C(=O)([O-])[O-].[Na+].[Na+].Cl[C:24]([O:26][CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)=[O:25]>O>[C:24]([N:2]1[C@@H:3]([C:14]([OH:16])=[O:15])[CH2:4][C:5]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[NH:7][C:6]=2[CH2:1]1)([O:26][CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)=[O:25]参加物
5
実験手順
5.00 g (3R)-1,2,3,4-Tetrahydro-9H-pyrido[3,4-b]-indole-3-carboxylic acid is suspended in 50 ml water/50 ml tetrahydrofuran and 5.15 g sodium carbonate is added. The mixture is stirred for 5 minutes and 3.94 g benzyl chloroformate is added and the mixture stirred overnight. The mixture is evaporated in vacuo to remove the THF, the aqueous residue acidified with 1N hydrochloric acid and the resulting solid extracted into ethyl acetate. The organic solution is washed with 1N HCl, water, brine, and dried over sodium sulfate. The solution is filtered, evaporated and the residue crystallized from toluene to give (3R)-2-carbobenzoxy-1,2,3,4-tetrahydro-9H-pyrido[3,4-b]indole-3-carboxylic acid, m.p. 181°-184° C.
後処理
- stirringthe mixture stirred overnight
- customThe mixture is evaporated in vacuo
- customto remove the THF
- extractionthe resulting solid extracted into ethyl acetate
- washThe organic solution is washed with 1N HCl, water, brine
- dry with materialdried over sodium sulfate
- filtrationThe solution is filtered
- customevaporated
- customthe residue crystallized from toluene
出典と根拠
- ORDレコード
- ord-a56da113337748c6a343aabaf1aa0260
- 出典データセット
- uspto-grants-1992_11
- 特許番号
- US05162336
関連ノート
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