반응 #3291

반응 방정식

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

3,4-methylenedioxyaniline

→

2-(Benzo[1,3]dioxol-5-ylamino)-6-(2,6-dichlorophenyl)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

용매

Ethyl acetate

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도The resulting solution was heated for 5 minutes
3. 3
   온도cooled to room temperature
4. 4
   여과some traces of solids were filtered
5. 5
   여과were filtered
6. 6
   세척washed with 2 mL of ethyl acetate
7. 7
   기타The solid was purified
8. 8
   기타to remove dark colors by silica gel chromatography
9. 9
   세척eluting with chloroform
10. 10
    기타50% hexane/ethyl acetate to obtain pure crystalline product

실험 절차

A mixture of 0.113 g (0.29 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.50 g (3.70 mmol) of 3,4-methylenedioxyaniline was heated, with stirring, in a 200° C. oil bath. The resulting solution was heated for 5 minutes and cooled to room temperature. Ethyl acetate (2 mL) was added, and some traces of solids were filtered. The crystals that slowly developed in the filtrate were filtered and washed with 2 mL of ethyl acetate; wt 0.080 g. The solid was purified to remove dark colors by silica gel chromatography, eluting with chloroform and then 50% hexane/ethyl acetate to obtain pure crystalline product; wt 0.054 g; mp 240°-241° C.

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