1,2-Dichloroethane → Ethyl 2-(4-acetyl-1-piperazinyl)-8-(2-chloroethyl)-5,8-dihydro-5-oxopyrido[2,3-d]-pyrimidine-6-carboxylate

HRID 1658130ノート

反応式

HRID 1658130 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[N:11]=[CH:12][C:13]3[C:19]([O:20]CC)=[C:18]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:17]=[N:16][C:14]=3[N:15]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[Cl:28][CH2:29][CH2:30]Cl>>[C:1]([N:4]1[CH2:5][CH2:6][N:7]([C:10]2[N:11]=[CH:12][C:13]3[C:19](=[O:20])[C:18]([C:23]([O:25][CH2:26][CH3:27])=[O:24])=[CH:17][N:16]([CH2:30][CH2:29][Cl:28])[C:14]=3[N:15]=2)[CH2:8][CH2:9]1)(=[O:3])[CH3:2]

参加物

3

反応物 2

HCID 111,2-DichloroethaneHCID 21532580Ethyl 2-(4-acetyl-1-piperazinyl)-5-ethoxypyrido[2,3-d]pyrimidine-6-carboxylate

生成物 1

HCID 13334740Ethyl 2-(4-acetyl-1-piperazinyl)-8-(2-chloroethyl)-5,8-dihydro-5-oxopyrido[2,3-d]-pyrimidine-6-carboxylate

実験手順

A solution of 1.0 g of ethyl 2-(4-acetyl-1-piperazinyl)-5-ethoxypyrido[2,3-d]pyrimidine-6-carboxylate in 10 ml of 1,2-dichloroethane was heated to reflux for 15 hours. After removal of an excess of the reagent by distillation, the resulting solid was taken up in chloroform and the chloroform solution washed with water, and dried over anhydrous magnesium sulfate. The solvent was distilled off to leave a solid which was recrystallized from ethyl acetate to give 0.65 g of the product, m.p. 205° - 206°C.

後処理

  1. temperatureto reflux for 15 hours
  2. customAfter removal of an excess of the reagent
  3. distillationby distillation
  4. washthe chloroform solution washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off
  7. customto leave a solid which
  8. customwas recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-ebac1a57b69148f284740b707792ea87
出典データセット
uspto-grants-1976_06
特許番号
US03962443

反応ノート

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