Water → Acesulfame

温度

40 °C

Different quantities of water were added to 150 ml of acetone. 10.1 g (0.1 mol) of acetoacetamide and 69 g (0.5 mol) of finely powdered, dry K2CO3 were added to each of these mixtures. 15.3 g (0.15 mol) of sulfuryl fluoride gas were then passed in--initially at room temperature. The temperature of the reaction mixture increased to about 40° C. during this process. The mixture was stirred for a further 2 hours and the product was filtered off with suction. The filter residue contained Acesulfam K, which was found to be identical to a reference sample by thin layer chromatography (silica gel, solvent system: ethyl acetate/glacial acetic acid 5:1). The filter residue was introduced into a mixture of excess hydrochloric acid with ice and extracted with ethyl acetate. The ethyl acetate extract was dried over Na2SO4 and evaporated in vacuo. Crystalline 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide was obtained and this was converted to Acesulfam K with methanolic KOH. The results are collated in the table which follows. In the last experiment listed in the table, the K2CO3 was used as a 50% aqueous solution.

1. custominitially at room temperature
2. filtrationthe product was filtered off with suction
3. additionThe filter residue was introduced into a mixture of excess hydrochloric acid with ice
4. extractionextracted with ethyl acetate
5. extractionThe ethyl acetate extract
6. dry with materialwas dried over Na2SO4
7. customevaporated in vacuo

ORDレコード

ord-33ff1ecc86574ef5813b5449befae66b

出典データセット

uspto-grants-1986_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04625024