5061-21-2 2-Bromo-4-butanolide 95463, aTetrahydrofurans compound, is more and more widely used in various fields.
5061-21-2, 2-Bromo-4-butanolide is a Tetrahydrofurans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
5061-21-2, [Example 1]; Production of 2-mercapto-4-butyrolactone; 49 g (0.6 mol) of 70% sodium hydrosulfide (manufactured by JUNSEI CHEMICAL Co., Ltd.) were dissolved in a mixture of 34 g of 1,2-dimethoxyethane (Guaranteed Reagent; manufactured by JUNSEI CHEMICAL CO., LTD.) and 34 g of purified water (which had been distilled and passed through an ion exchange filter) at room temperature. While the resultant solution was cooledwith ice (to 100C or less) and under normal pressure (about 0.10MPa), 18 g of hydrochloric acid (GUARANTEED REAGENT, 35%to 37%; manufactured by JUNSEI CHEMICAL Co., Ltd.) were addedwith stirring the solution to adjust the pH of the solution to8.9. While the solution was maintained at a temperature of 100C or less, 34 g (0.2 mol) of 2-bromo-4-butyrolactone (manufacturedby Tokyo Chemical Industry Co., Ltd.) were added dropwise intothe solution over approximately 20 minutes. The reaction solution after the completion of the dropwise addition was stirred for 2 minutes . The pH of the reaction solution was withinthe range of 7.5 to 8.9 from when the dropwise addition of 2-bromo-4-butyrolactone was initiated to the stirring after thedropwise addition was completed. [0077]Thereafter, while the solution was cooled at 100C or less, 24 g of hydrochloric acid were added to the solution overapproximately 5 minutes to adjust the pH of the solution to 4.0. An inorganic salt precipitated in the solution was removed by suction filtration, and 20 g of ethyl acetate (GUARANTEED REAGENT; manufactured by JUNSEI CHEMICAL Co., Ltd.) were added to the resultant filtrate to extract the organic phase. The resultant aqueous phase was reextracted with 34 g of ethyl acetate. These extracted organic phases were combined. The organic phase was concentrated and purified by distillationunder a reduced pressure to give 19 g of2-mercapto-4-butyrolactone (having a boiling point of 94C/0.3 kPa; with a yield of 78%) .; [Examples 33 to 36]; In substantially the same manner as in Example 1 except that the temperature of the reaction solution during the reaction was changed as described in Table 4, the reaction was performed to synthesize 2-mercapto-4-butyrolactone. The results are shown in Table 4. The SH reaction yields in Table4 were calculated from the HPLC analysis results of samples which had been picked up from the reaction solution when the pH of the reaction solution was adjusted to 4.0.
5061-21-2 2-Bromo-4-butanolide 95463, aTetrahydrofurans compound, is more and more widely used in various fields.
Reference£º
Patent; SHOWA DENKO K.K.; WO2007/139215; (2007); A1;,
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