反応式
[NH2:1][C@@H:2]1[CH2:7][CH2:6][CH2:5][C@H:4]([NH:8][C:9](=[O:18])[O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:3]1.Cl[C:20]([O:22][CH3:23])=[O:21].C(N(CC)CC)C>C1COCC1>[CH2:11]([O:10][C:9]([NH:8][C@H:4]1[CH2:5][CH2:6][CH2:7][C@@H:2]([NH:1][C:20](=[O:21])[O:22][CH3:23])[CH2:3]1)=[O:18])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1参加物
5
実験手順
Benzyl N-[(1S,3R)-3-aminocyclohexyl]carbamate, 18e, (0.99 g, 3.99 mmol) was dissolved in THF (20 mL) and treated with methyl chloroformate (0.62 mL, 7.97 mmol), followed by triethylamine (1.67 mL, 11.96 mmol). After stirring for 1 hour at room temperature, the solvent was evaporated under reduced pressure and the residue was diluted into 1:3 mixture of CH2Cl2:EtOAc (130 mL) and washed with 1N HCl (50 mL) and 2N Na2CO3 (50 mL). The organic layer was dried over Na2SO4 and concentrated under reduced pressure to afford the desired product, 19a, as a white solid (1.09 g, 89% yield).
後処理
- customthe solvent was evaporated under reduced pressure
- additionthe residue was diluted into 1:3 mixture of CH2Cl2
- washEtOAc (130 mL) and washed with 1N HCl (50 mL) and 2N Na2CO3 (50 mL)
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-55bcb3c49562482bb9f7303c3618d05e
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09345708B2
関連ノート
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