反応 #3307

反応方程式

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-(hydroxymethyl)aniline

acetic acid

→

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

溶媒

Water

反応条件

後処理

1. 1
   workup.DISSOLUTIONto dissolve the gum
2. 2
   その他to precipitate a solid
3. 3
   ろ過The mixture was filtered
4. 4
   洗浄The cake was washed well with water
5. 5
   その他dried
6. 6
   その他Purification
7. 7
   洗浄eluting with chloroform
8. 8
   その他with ethyl acetate to obtain the fraction
9. 9
   workup.ADDITIONcontaining the pure product
10. 10
    濃縮The ethyl acetate eluent was concentrated to 1 mL volume
11. 11
    その他The crystals that separated one inducement
12. 12
    ろ過were filtered
13. 13
    洗浄washed with 0.5 mL of ethyl acetate

実験手順

A mixture of 0.155 g (0.40 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.500 g (4.10 mmol) of 3-(hydroxymethyl)aniline was heated in a 180° C. oil bath for 10 minutes. At ca. 120° C., 2 mL of glacial acetic acid were added to dissolve the gum. Water (20 mL) was added to precipitate a solid. The mixture was filtered. The cake was washed well with water and dried; wt 0.130 g. Purification was effected by silica gel chromatography eluting with chloroform and then with ethyl acetate to obtain the fraction containing the pure product. The ethyl acetate eluent was concentrated to 1 mL volume. The crystals that separated one inducement were filtered and washed with 0.5 mL of ethyl acetate and then 1 mL of ether; wt 0.059 g; mp 215°-217° C.

出典