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Carbamic acid, N-(2-oxo-3-buten-1-yl)-, phenylmethyl ester synthesis

2synthesis methods
-

Yield:-

Reaction Conditions:

in tetrahydrofuran;dichloromethane at 0;

Steps:

27 Synthesis of Compound 27 benzyl 2-oxobut-3-enylcarbamate

Example 27 Synthesis of Compound 27 benzyl 2-oxobut-3-enylcarbamate To the Weinreb amide 26 (3.89 g, 15.42 mmol) in DCM (lOmL) at 0° C. was added vinyl magnesium bromide (45 mmol) in THF (45 mL). The reaction was stirred for 2 hrs and monitored by HPLC. The reaction was added to a mixture of ice and 1 M hydrochloric acid (200 mL). The aqueous mixture was extracted with DCM (3*100 mL) and washed with 1M hydrochloric acid (2*200 mL) and H2O (3*100 mL). The organic phase was dried (MgSO4) and the volume reduced to 100 mL by rotary evaporation. The α,β-unsaturated ketone 27 was stored and used in solution without purification.

References:

US2009/221557,2009,A1 Location in patent:Page/Page column 119