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With hydrogen;palladium 10% on activated carbon; In methanol; under 2585.81 Torr; for 1h;
The acid prepared in Step A (230 g, 1.0 mol) and 10 % Pd/C (5.0 G) in 500 ML of methanol on a Parr shaker was HYDROGENATED under 50 psi of hydrogen for 1 h. The catalyst was removed by filtration and the filtrate was evaporated. The residue was dissolved in dichloromethane and dried over anhydrous sodium sulfate. After filtration, the filtrate was evaporated and dried under vacuum. The title compound was obtained as a light yellow solid (230 g, 99 %). LC-MS for C11H19N04 [M+H+] CALCULATED 230, found 230.
99%
With hydrogen;palladium 10% on activated carbon; In methanol; for 1h;
The acid (Step A, Procedure A, Intermediate 5) (227 g, 1.0 mol) and 10% Pd/C (5.0 g) in 500 mL of methanol on a Parr shaker was hydrogenated under 50 lb of hydrogen for one hour. The catalyst was removed by filtration and the filtrate was evaporated. The residue was dissolved in dichloromethane and dried over anhydrous sodium sulfate. After filtered, the filtrate was evaporated and dried in vacuum. The title compound was obtained as a light yellow solid (226.0 g, 99 %). LC-MS for C1 lH19NO4 [MF calculated 230, found 230.
99%
With hydrogen;palladium 10% on activated carbon; In methanol; under 2585.81 Torr; for 1h;Product distribution / selectivity;
Step B; The solution of the acid (Step A, Procedure A, Intermediate 4) (227 g, 1.0 mol) and 10% Pd/C (5.0 g) in 500 mL of methanol was hydrogenated under 50 lb of hydrogen for one hour. The catalyst was removed by filtration and the filtrate was evaporated to dryness. The residue was dissolved in dichloromethane and dried over anhydrous sodium sulfate. The filtrate was evaporated to dryness and dried in vacuum. The title compound was obtained as a light yellow solid (226.0 g, 99%). LC-MS for C11H19NO4 [M+H+] calculated 230, found 230.; Step B The acid prepared in Step A (230 g, 1.0 mol) and 10% Pd/C (5.0 g) in 500 mL of methanol was placed on a Parr apparatus and hydrogenated under 50 psi of hydrogen for 1 h. The catalyst was removed by filtration and the filtrate was evaporated. The residue was dissolved in dichloromethane and dried over anhydrous sodium sulfate. After filtration, the filtrate was evaporated and dried under vacuum. The title compound was obtained as a light yellow solid (230 g, 99%). LC-MS for C11H19NO4 calculated 229, found [M+H]+ 230.
99%
With hydrogen;palladium 10% on activated carbon; In methanol; for 1h;
The acid (Step A, Procedure A, Intermediate 5) (227 g, 1.0 mol) and 10% Pd/C (5.0 g) in 500 mL of methanol on a Parr shaker was hydrogenated under 50 lb of hydrogen for one hour. The catalyst was removed by filtration and the filtrate was evaporated. The residue was dissolved in dichloromethane and dried over anhydrous sodium sulfate. After filtered, the filtrate was evaporated and dried in vacuum. The title compound was obtained as a light yellow solid (226.0 g, 99 %). LC-MS for C11H19NO4 [M+H+] calculated 230, found 230.
With hydrogen;5%-palladium/activated carbon; In ethyl acetate; at 20℃; under 2068.65 Torr; for 3h;Product distribution / selectivity;
Step 2; (lS, 3R)- (+)-3-N-BOC-Aminocyclopentane-l-carboxylic acid; To a solution of Step 1 intermediate (8.0 g, 35.2 mmol) in ethyl acetate (150 ml) was added 5 % Pd- C (1.0 g) and the mixture was maintained under hydrogen pressure (40 psi) for 3 h at RT to give 8. 0 g of the product as a white solid, which was identical in all respects with the product obtained from Method A.
With hydrogen;5%-palladium/activated carbon; In ethyl acetate; at 20℃; under 2068.65 Torr; for 3h;Product distribution / selectivity;
To a solution of Step 1 intermediate, from Method A, Intermediate 5 (8.0 g, 35.2 mmol) in ethyl acetate (150 ml) was added 5 % Pd/C (1.0 g) and the mixture was maintained under hydrogen pressure (40 psi) for 3 h at room temperature to give 8.0 g of the product as a white solid, which was identical in all respects with the product obtained from Method A.
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