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ChemicalBook CAS DataBase List 1-Boc-3-cyano-4-oxopyrrolidine
175463-32-8

1-Boc-3-cyano-4-oxopyrrolidine synthesis

7synthesis methods
266353-18-8 Synthesis
N-BOC-N-(2-CYANOETHYL) GLYCINE ETHYL ESTER

266353-18-8
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Yield:175463-32-8 68%

Reaction Conditions:

with sodium in ethanol for 1 h;Reflux;

Steps:

1 Synthesis of 4-cyano-1- (N-tert-butoxycarbonyl) pyrrolidin-3-one (3)
The oil 2 was dissolved in 50 mL of absolute ethanol,The solution was added dropwise to a solution of 4 g (0.17 mol) of metallic sodium in 100 mL of absolute ethanol under reflux with heating,Refluxed for 1 h.The solvent was distilled off under reduced pressure, and the residue was treated with 100 mLWater was dissolved and washed with ethyl acetate (30 mL * 2). The aqueous layer was adjusted to pH 4 with 1 mol / L hydrochloric acid, extracted with ethyl acetate,Dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated to a residual solvent of about 20 mL, filtered and the cake washed with a small amount of ethyl acetateDry cake to give 16.5 g of a white solid. Yield: 68%.

References:

Huaren Pharmaceutical Co Ltd;Guo, Jin;Feng, Xinguang;Han, Yong;Jiang, Ming;Li, Jiren;Zou, Shanshan CN105585518, 2016, A Location in patent:Paragraph 0024; 0026

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