反応式
[C:1]([O:5][C:6](=[O:34])[C:7](=[CH:19][C:20]1[CH:25]=[CH:24][N:23]=[C:22]([NH:26][C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH:21]=1)[CH2:8][C:9]([O:11]CC1C=CC=CC=1)=[O:10])([CH3:4])([CH3:3])[CH3:2]>CCO.[Pd]>[C:1]([O:5][C:6](=[O:34])[CH:7]([CH2:19][C:20]1[CH:25]=[CH:24][N:23]=[C:22]([NH:26][C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH:21]=1)[CH2:8][C:9]([OH:11])=[O:10])([CH3:4])([CH3:3])[CH3:2]参加物
実験手順
2-(2-tert-Butoxycarbonylamino-pyridin-4-ylmethylene)-succinic acid 4-benzyl ester 1-tert-butyl ester (2.81 g, 7.60 mmol) and Pd/C (10%, 400 mg) were suspended in EtOH and hydrogenated at 41 atm. and 28° C. for 3 days. The catalyst was removed from the reaction mixture by filtration. The catalyst was washed with EtOH (96%). 1 M K2CO3 (30 mL) was added to the filtrate followed by addition of water (50 mL). After 2 days the reaction mixture was evaporated to ca 80 mL, then brine (10 mL) was added and the reaction mixture extracted with ether. The aqueous phase was acidified to pH=3 and extracted with chloroform. Methanol (25 mL) was added and the reaction mixture was dried (Na2SO4+CaSO4) and filtered to give 2-(2-tert-butoxycarbonylamino-pyridin-4-ylmethyl)-succinic acid 1-tert-butyl ester (1.90 g, 83%).
後処理
- customThe catalyst was removed from the reaction mixture by filtration
- washThe catalyst was washed with EtOH (96%)
- addition1 M K2CO3 (30 mL) was added to the filtrate
- additionfollowed by addition of water (50 mL)
- customAfter 2 days the reaction mixture was evaporated to ca 80 mL
- additionbrine (10 mL) was added
- extractionthe reaction mixture extracted with ether
- extractionextracted with chloroform
- additionMethanol (25 mL) was added
- dry with materialthe reaction mixture was dried (Na2SO4+CaSO4)
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-7f8f1cafed2747709f9692ed7b1bdb9f
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07354895B1
関連ノート
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