反应详情

To a 30 L reaction kettle was added 4 L dry THF at −10° C. After stirring, to the mixture were added ZnCl2 (118 g, 0.86 mol) and LiCl (402 g, 9.5 mol). After half an hour, to the resulting mixture was slowly added dropwisely a solution of MeMgBr (3 mol/L) in diethyl ether (6.4 L, 19.2 mol). The stirring was continued for half an hour. To the resulting mixture was slowly added a solution of tert-butyl 3-oxopyrrolidine-1-carboxylate (1600 g, 8.6 mol) in THF dropwisely. After the completion of reaction by HPLC detection, to the system was dropwisely added a saturated NH4Cl solution to quench off the reaction. The reaction was extracted with ethyl acetate. The organic phase was washed with a saturated aqueous NaCl solution, dried over anhydrous sodium sulfate, and evaporated to remove the solvent to produce tert-butyl 3-hydroxy-3-methylpyrrolidine-1-carboxylate as a pale-yellow solid (1450 g) in a yield of 83.8%.

1. customTo a 30 L reaction kettle
2. waitAfter half an hour
3. waitThe stirring was continued for half an hour
4. customAfter the completion of reaction by HPLC detection
5. customto quench off
6. customthe reaction
7. extractionThe reaction was extracted with ethyl acetate
8. washThe organic phase was washed with a saturated aqueous NaCl solution
9. dry with materialdried over anhydrous sodium sulfate
10. customevaporated
11. customto remove the solvent