Acetic Acid → PD-166326

HRID 3211

反応式

HRID 3211 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:22](=[O:23])[N:21]([CH3:24])[C:12]2[N:13]=[C:14](S(C)(=O)=O)[N:15]=[CH:16][C:11]=2[CH:10]=1.[OH:25][CH2:26][C:27]1[CH:28]=[C:29]([CH:31]=[CH:32][CH:33]=1)[NH2:30].C(O)(=O)C>O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:22](=[O:23])[N:21]([CH3:24])[C:12]2[N:13]=[C:14]([NH:30][C:29]3[CH:31]=[CH:32][CH:33]=[C:27]([CH2:26][OH:25])[CH:28]=3)[N:15]=[CH:16][C:11]=2[CH:10]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 802933-Aminobenzyl alcoholHCID 105961576-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one

生成物 1

HCID 447700PD-166326

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
180 °C

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.

後処理

  1. dissolutionto dissolve the gum
  2. customto precipitate a solid
  3. filtrationThe mixture was filtered
  4. washThe cake was washed well with water
  5. customdried
  6. customPurification
  7. washeluting with chloroform
  8. customwith ethyl acetate to obtain the fraction
  9. additioncontaining the pure product
  10. concentrationThe ethyl acetate eluent was concentrated to 1 mL volume
  11. customThe crystals that separated one inducement
  12. filtrationwere filtered
  13. washwashed with 0.5 mL of ethyl acetate

出典と根拠

ORDレコード
ord-4b3709d670944052a53ca165365f8b96
出典データセット
uspto-grants-1998_03
特許番号
US05733914

関連ノート

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