Hydrochloric Acid → 6-(2-bromo-6-chlorophenyl)-8-ethyl-2-phenylamino-8H-pyrido[2,3-d]pyrimidin-7-one

HRID 3226ノート

反応式

HRID 3226 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:25](=N)[N:24]([CH2:27][CH3:28])[C:12]2[N:13]=[C:14]([NH:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[N:15]=[CH:16][C:11]=2[CH:10]=1.C(OC(=O)C)(=[O:31])C.Cl>O>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:25](=[O:31])[N:24]([CH2:27][CH3:28])[C:12]2[N:13]=[C:14]([NH:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[N:15]=[CH:16][C:11]=2[CH:10]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 18934792HCID 18934792、化合物

生成物 1

HCID 115833536-(2-bromo-6-chlorophenyl)-8-ethyl-2-phenylamino-8H-pyrido[2,3-d]pyrimidin-7-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

(6-(2-Bromo-6-chlorophenyl)-8-ethyl-7-imino-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-yl)-phenylamine (150 mg) was added to 1 mL of acetic anhydride and heated at reflux for 5 minutes. The reaction was cooled and concentrated resulting in an oil which was heated at reflux with 10 mL of 6N HCl for 10 minutes. The reaction was cooled, and 30 mL of water was added causing precipitation. The precipitate was removed by filtration and washed with water. The resulting solid was dried to give 130 mg of 6-(2-bromo-6-chlorophenyl)-8-ethyl-2-phenylamino-8H-pyrido[2,3-d]pyrimidin-7-one; mp softens at 195° C. and melts at 210°-214° C.

後処理

  1. temperatureheated
  2. temperatureat reflux for 5 minutes
  3. temperatureThe reaction was cooled
  4. concentrationconcentrated
  5. customresulting in an oil which
  6. temperaturewas heated
  7. temperatureThe reaction was cooled
  8. customprecipitation
  9. customThe precipitate was removed by filtration
  10. washwashed with water
  11. customThe resulting solid was dried

出典と根拠

ORDレコード
ord-8101dbefc33b4ad5952d74a7f2f862b6
出典データセット
uspto-grants-1998_03
特許番号
US05733914

反応ノート

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