4-Aminobenzonitrile → 7-Acetoxy-4-(4-cyanoanilino)-6,7-dihydro-5H-cyclopenta[d]pyrimidine

HRID 579747노트

반응식

HRID 579747 반응식
[C:1]([O:4][CH:5]1[C:9]2[N:10]=[CH:11][N:12]=[C:13](Cl)[C:8]=2[CH2:7][CH2:6]1)(=[O:3])[CH3:2].[NH2:15][C:16]1[CH:23]=[CH:22][C:19]([C:20]#[N:21])=[CH:18][CH:17]=1>C(O)C>[C:1]([O:4][CH:5]1[C:9]2[N:10]=[CH:11][N:12]=[C:13]([NH:15][C:16]3[CH:23]=[CH:22][C:19]([C:20]#[N:21])=[CH:18][CH:17]=3)[C:8]=2[CH2:7][CH2:6]1)(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 133964-AminobenzonitrileHCID 199689354-chloro-6,7-dihydro-5H-cyclopenta[d]pyrimidin-7-yl acetate

생성물 1

HCID 139132267-Acetoxy-4-(4-cyanoanilino)-6,7-dihydro-5H-cyclopenta[d]pyrimidine수율 55.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

39.3 g of 7-acetoxy-4-chloro-6,7-dihydro-5H-cyclopenta[d]pyrimidine [prepared as described in step (b) above] and 24 g of p-aminobenzonitrile were dissolved in 180 ml of ethanol, and the solution was heated under reflux for 1.5 hours. At the end of this time, the solvent was evaporated off under reduced pressure, and the resulting residue was washed with a 1:1 by volume mixture of ethanol and toluene, to give 30 g of the title compound as pale grayish crystals, melting at 215°-217° C.

후처리

  1. temperaturethe solution was heated
  2. temperatureunder reflux for 1.5 hours
  3. customAt the end of this time, the solvent was evaporated off under reduced pressure
  4. washthe resulting residue was washed with a 1:1 by volume mixture of ethanol and toluene

출처 및 근거

ORD 기록
ord-064491002d1040118ff9c94364c8cb47
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04749704

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