* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With dimethylsulfide borane complex; In tetrahydrofuran; at 0 - 20℃; for 2.0h;Inert atmosphere;
(2) room temperature and nitrogen protection,Compound 2 was dissolved in 700 mL of THF,Cooling to 0 ,Began to slowly add 345mL B2H6.Me2S, with bubbles,1h after the drop is completed, the system was green turbidity,Natural recovery to room temperature reaction 1h,System cooling to 0 ,To the system slowly add 500mL methanol quenching,Then returned to room temperature,45 water pump and pump concentrated dry.Vacuum distillation, external temperature 150 ,The temperature of 60 began to produce products.Outside the temperature of 160 , the temperature of 110 -120 stable product to the end,Distilled to give 16 g of product (Compound 3).
4.7 g
With lithium aluminium tetrahydride; In tetrahydrofuran; at -40 - -30℃; for 3.0h;Inert atmosphere;
In a 100 mL reaction flask equipped with a stirrer, 6.5 g of beta-carboxy-gamma-butyrolactone was added to 50 mL of anhydrous tetrahydrofuran and the reaction system was protected by nitrogen. The temperature was lowered to -40 C and 50 ml of thioether solution dissolved with lithium aluminum hydride 7g was slowly added dropwise to control the dropping rate so that the temperature of the reaction system was maintained at about -30 C. After the reaction was continued for 1 hour, the reaction was continued for 2 hours. The reaction of the raw materials was complete. 100 mL of ice water was added to the reaction mixture to quench the reaction, and the reaction mixture was extracted twice with 200 mL of ethyl acetate. The organic phases were combined and concentrated to give 4.7 g of beta-hydroxymethyl-gamma-butyrolactone.
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
120K+ Compounds
Competitive Price
1-2 Day Shipping
