反应详情

To 1.0 g. of 7-chloro-4-(4-chlorophenyl)-2-(hydroxymethyl)-5H-pyrido[3,4-b][1,4]benzothiazin-3(2H)-one (2.6 mmol.) in 15 ml. of pyridine at 0° C. was added dropwise 0.9 ml. of hexadecanoyl chloride (3.9 mmol.). After stirring for 35 minutes, the mixture was poured onto ice-water and allowed to stand for 16 hours at room temperature, resulting in the formation of a yellow precipitate. The precipitate was collected, washed with water and air-dried, then purified using flash chromatography on silica gel, employing a mixture of 2% ethyl acetate: 98% methylene chloride as the eluent. Fractions containing the product were combined and triturated with ether to yield 7-chloro-4-(4-chlorophenyl)-2-[(1-oxohexadecyloxy)methyl]-5H-pyrido[3,4-b][1,4]benzothiazin-3(2H)-one as a pale yellow crystalline solid (1.25 g; 78% yield) having the structural formula, ##STR21## a melting point in the range of 120°-122° C. and the following elemental analysis:

1. additionthe mixture was poured onto ice-water
2. waitto stand for 16 hours at room temperature
3. customresulting in the formation of a yellow precipitate
4. customThe precipitate was collected
5. washwashed with water
6. customair-dried
7. custompurified
8. additiona mixture of 2% ethyl acetate
9. additionFractions containing the product
10. customtriturated with ether