tert-Butanol → HCID 23070937、化合物
反応式
C([N:4]([CH:7](C)C)CC)(C)C.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:17])C=CC=CC=1.[C:27]([OH:31])([CH3:30])([CH3:29])[CH3:28].C([CH:35]1[CH2:40][CH2:39][CH2:38][N:37]([C:41]([O:43][CH2:44][CH:45]2[C:57]3[CH:56]=[CH:55][CH:54]=[CH:53][C:52]=3[C:51]3[C:46]2=[CH:47][CH:48]=[CH:49][CH:50]=3)=[O:42])[CH2:36]1)(O)=O>C(OCC)(=O)C>[C:27]([O:31][C:7]([NH:4][CH:35]1[CH2:40][CH2:39][CH2:38][N:37]([C:41]([O:43][CH2:44][CH:45]2[C:57]3[CH:52]=[CH:53][CH:54]=[CH:55][C:56]=3[C:47]3[C:46]2=[CH:51][CH:50]=[CH:49][CH:48]=3)=[O:42])[CH2:36]1)=[O:17])([CH3:30])([CH3:29])[CH3:28]参加物
反応条件
- 温度
- 60 °C
実験手順
1.84 g of diisopropylethylamine and 4.71 g of diphenylphosphorylazide were added to 10 ml of a t-butanol solution of 5.01 g of 9H-fluoren-9-ylmethyl 3-carboxypiperidine-1-carboxylate, and the mixture was heated at 60° C. under a nitrogen atmosphere for 18 hours. The reaction solution was cooled, and 150 ml of ethyl acetate was added thereto. The organic layer was washed successively with 100 ml of 5% aqueous sulfuric acid, 100 ml of 5% aqueous sodium bicarbonate solution, 100 ml of water, and 100 ml of a saturated sodium chloride solution, and then dried over anhydrous magnesium sulfate. The organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography. Thus, 1.88 g of the title compound was obtained from the fraction eluted with hexane-ethyl acetate (4:1).
後処理
- temperatureThe reaction solution was cooled
- washThe organic layer was washed successively with 100 ml of 5% aqueous sulfuric acid, 100 ml of 5% aqueous sodium bicarbonate solution, 100 ml of water, and 100 ml of a saturated sodium chloride solution
- dry with materialdried over anhydrous magnesium sulfate
- concentrationThe organic layer was concentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-6ad8e6360506424e81355a2eeb32dacd
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07772226B2
反応ノート
読み込み中…