반응 #3299

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-methyl-4-methoxyaniline

→

6-(2,6-Dichlorophenyl)-2-(4-methoxy-3-methylphenylamino)-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one

용매

Ether

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
   여과The crystals that developed were filtered
5. 5
   세척washed with 2 mL of ether
6. 6
   기타The solid was purified
7. 7
   기타to remove dark colors by silica gel chromatography
8. 8
   세척eluting with chloroform
9. 9
   농축The ethyl acetate eluent was concentrated to 3 mL volume
10. 10
    온도On cooling
11. 11
    기타pure crystals of product separated

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 0.40 g (2.90 mmol) of 3-methyl-4-methoxyaniline was heated, with stirring, in a 165° C. oil bath. The resulting solution was heated for 5 minutes and cooled to room temperature. Ether (1 mL) was added. The crystals that developed were filtered and washed with 2 mL of ether; wt 0.109 g. The solid was purified to remove dark colors by silica gel chromatography, eluting with chloroform and then ethyl acetate. The ethyl acetate eluent was concentrated to 3 mL volume. On cooling, pure crystals of product separated; wt 0.060 g; mp 218°-220° C.

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