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

HRID 1658130노트

반응식

HRID 1658130 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ebac1a57b69148f284740b707792ea87
출처 데이터셋
uspto-grants-1976_06
특허 번호
US03962443

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