2-Bromo-4-butanolide synthesis

4synthesis methods

Product Name:2-Bromo-4-butanolide
CAS Number:5061-21-2
Molecular formula:C4H5BrO2
Molecular Weight:164.99

96-48-0

5061-21-2

General procedure for the synthesis of α-bromo-γ-butyrolactone from γ-butyrolactone (bromination step): in a 1000 mL reaction vessel equipped with a stirring device, refluxing device, thermometer, dropping funnel, and nitrogen introduction tube, 200 g (2.32 mol) of γ-butyrolactone and 2.76 g (0.086 mol based on 3.7 mol% of γ-butyrolactone) of sulfur were added as the catalyst. 431 g (2.70 mol) of bromine was loaded into a dropping funnel. Stirring was initiated, the reaction temperature was controlled not to exceed 40 °C, and the bromine was slowly added dropwise. After the dropwise addition was completed, the reaction temperature was raised to about 90 °C and the reaction was maintained at this temperature for 1 hour. Subsequently, the temperature was raised to about 110°C and the reaction was continued for 3 hours.

96-48-0
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5061-21-2
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$25.00/5G

Yield:5061-21-2 93.1%

Reaction Conditions:

with sulphur;bromine at 40 - 110; for 4 h;Inert atmosphere;Temperature;Reagent/catalyst;

Steps:

1-3; 1; 2 [Example 1]

(Bromination step) A stirring device, a reflux device, a thermometer,In a reaction vessel equipped with a dropping funnel and a nitrogen introducing tube and having a volume of 1000 ml,200 g (2.32 mol) of γ-butyrolactone,And catalyst as sulfur 2.76g (0.086mol,3.7 mol% based on γ-butyrolactone)431 g (2.70 mol) of bromine was charged into the dropping funnel.Stirring was started,While keeping the temperature inside the reaction container not to exceed 40 ° C.,The whole amount of bromine in the dropping funnel was dropped.After completion of the dropwise addition,The temperature inside the reaction vessel was raised to about 90 ° C. and the reaction vessel was heated for 1 hour,Then, the temperature was raised to about 110 ° C. and the reaction was carried out for 3 hours.

References:

JP5837752,2015,B2 Location in patent:Paragraph 0052; 0079-0081; 0082; 0085; 0086; 0088