تفاعل #3312

معادلة التفاعل

6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

6-(2,6-Dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

3-aminobenzoic acid, ethyl ester

acetic acid

→

3-[6-(2,6-Dichlorophenyl)-8-methyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino]-benzoic acid, ethyl ester

المذيبات

Water

ظروف التفاعل

المعالجة

1. 1
   أخرىwas fused in a 170° C.
2. 2
   أخرىto give a clear melt
3. 3
   workup.DISSOLUTIONto dissolve the melt
4. 4
   أخرىto precipitate a solid
5. 5
   ترشيحThe solid was filtered
6. 6
   غسيلwashed well with water
7. 7
   أخرىtriturated with 2 mL of methanol
8. 8
   ترشيحThe mixture was filtered
9. 9
   غسيلthe cake was washed with 1 mL of methanol
10. 10
    أخرىRecrystallization from ethyl acetate
11. 11
    أخرىgave pure product

الإجراء التجريبي

A mixture of 0.226 g (0.58 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.40 g (2.42 mmol) of 3-aminobenzoic acid, ethyl ester was fused in a 170° C. oil bath to give a clear melt. After 6 minutes, the melt was cooled to ca. 100° C. Glacial acetic acid (1 mL) was added to dissolve the melt. Water (5 mL) was added to precipitate a solid. The solid was filtered, washed well with water, and triturated with 2 mL of methanol. The mixture was filtered, and the cake was washed with 1 mL of methanol and then ether; wt 0.194 g. Recrystallization from ethyl acetate gave pure product; wt 0.075 g; mp 238°-240° C.

المصدر