Toluene → 2-(4'-Benzyl-piperazino)-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydro-pyrido(2,3-d)pyrimidine

HRID 66002노트

반응식

HRID 66002 반응식
Cl[C:2]1[N:3]=[CH:4][C:5]2[C:11](=[O:12])[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:9][N:8]([CH2:18][CH3:19])[C:6]=2[N:7]=1.[CH2:20]([N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C1(C)C=CC=CC=1>C(Cl)(Cl)Cl.O>[CH2:20]([N:27]1[CH2:32][CH2:31][N:30]([C:2]2[N:3]=[CH:4][C:5]3[C:11](=[O:12])[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:9][N:8]([CH2:18][CH3:19])[C:6]=3[N:7]=2)[CH2:29][CH2:28]1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

참가 물질

6

반응물 3

HCID 1140TolueneHCID 759941-BenzylpiperazineHCID 122668052-Chloro-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydropyrido(2,3-d)pyrimidine

생성물 1

HCID 122668082-(4'-Benzyl-piperazino)-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydro-pyrido(2,3-d)pyrimidine수율 90%

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

As described in Example VI, a mixture of 5.6 g. of 2-chloro-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydropyrido(2,3-d)pyrimidine, 7.04 g. of N-benzylpiperazine and 80 cm3 of toluene is heated under reflux for 2 hours. After cooling, the mass is diluted with 100 cm3 of chloroform and is taken up in 200 cm3 of water. After washing the organic phase with water, the reaction product is isolated as described in the Example mentioned. It is recrystallised from isopropanol. 7.6 g. (90%) of 2-(4'-benzyl-piperazino)-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydro-pyrido(2,3-d)pyrimidine are obtained; melting point 152° C.

후처리

  1. additiona mixture of 5.6 g
  2. temperatureunder reflux for 2 hours
  3. temperatureAfter cooling
  4. washAfter washing the organic phase with water
  5. customthe reaction product is isolated
  6. customIt is recrystallised from isopropanol

출처 및 근거

ORD 기록
ord-fa47c2ad0e9e443182fecb169b01b9ea
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04129737

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