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

HRID 867183노트

반응식

HRID 867183 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])[C:18]([C:21]([O:23]CC)=[O:22])=[CH:17][NH:16][C:14]=3[N:15]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]>Cl.C(O)C>[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])[C:18]([C:21]([OH:23])=[O:22])=[CH:17][NH:16][C:14]=3[N:15]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

참가 물질

4

반응물 1

HCID 12917681Ethyl 2-(4-acetyl-1-piperazinyl)-5,8-dihydro-5-oxopyrido[2,3-d]pyrimidine-6-carboxylate

생성물 1

HCID 128507552-(4-Acetyl-1-piperazinyl)-5,8-dihydro-5-oxopyrido[2,3-d]pyrimidine-6-carboxylic acid수율 54.4%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

반응 조건

온도
120 °C

실험 절차

A suspension of ethyl 5,8-dihydro-2-(4-acetyl-1-piperazinyl)-5-oxopyrido[2,3-d]pyrimidine-6-carboxylate (20 g) in a mixture of 4% hydrochloric acid (60 ml) and ethanol (20 ml) was refluxed at 120° C. for 1.5 hours. After cooling, the precipitate was collected, washed with water and then with hot water, and dissolved in a 10% sodium hydroxide solution. The insoluble material was filtered off and the filtrate was acidified with diluted hydrochloric acid. The resulting precipitate was collected and recrystallized from dimethyl sulfoxide to give 5,8-dihydro-2-(4-acetyl-1-piperazinyl)-5-oxopyrido[2,3-d]pyrimidine-6-carboxylic acid (10 g). m.p. 298°-300° C.

후처리

  1. temperatureAfter cooling
  2. customthe precipitate was collected
  3. washwashed with water
  4. dissolutionwith hot water, and dissolved in a 10% sodium hydroxide solution
  5. filtrationThe insoluble material was filtered off
  6. customThe resulting precipitate was collected
  7. customrecrystallized from dimethyl sulfoxide

출처 및 근거

ORD 기록
ord-4c2bf0d2c03a4507bc8a16b771cd3c40
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04103011

반응 노트

불러오는 중…