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HCID 178468507, 화합물 → Ethyl 2-amino-4-(4-fluorophenyl)-6-(propan-2-yl)pyrimidine-5-carboxylate

HRID 2390757
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HRID 2390757 반응식
[NH2:1][C:2]1[NH:3][CH:4]([CH:20]([CH3:22])[CH3:21])[C:5]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][CH:9]=2)[N:7]=1>C1(C)C=CC=CC=1.[O-2].[O-2].[Mn+4]>[NH2:1][C:2]1[N:7]=[C:6]([C:8]2[CH:9]=[CH:10][C:11]([F:14])=[CH:12][CH:13]=2)[C:5]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[C:4]([CH:20]([CH3:21])[CH3:22])[N:3]=1
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참가 물질

4

반응물 1

HCID 178468507HCID 178468507, 화합물

생성물 1

HCID 24987285Ethyl 2-amino-4-(4-fluorophenyl)-6-(propan-2-yl)pyrimidine-5-carboxylate수율 96%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 1140Toluene용매2회

실험 절차

Ethyl 2-amino-4-(4-fluorophenyl)-6-isopropyl-1,6-dihydropyrimidine-5-carboxylate (22.6 g) was dissolved in toluene (150 ml) and heated until a solution was obtained. Manganese dioxide (18.8 g) was added as a slurry in toluene (150 ml) and the mixture refluxed under azeotropic conditions for 6 hours until conversion was complete. A small amount of water was collected in the Dean and Stark trap. The slurry was filtered and the solvents removed by evaporation under reduced pressure to give ethyl 2-amino-4-(4-fluorophenyl)-6-isopropyl-pyrimidine-5-carboxylate as a crystalline solid in 96% yield.

후처리

  1. temperatureheated until a solution
  2. customwas obtained
  3. temperaturethe mixture refluxed under azeotropic conditions for 6 hours until conversion
  4. customA small amount of water was collected in the Dean and Stark trap
  5. filtrationThe slurry was filtered
  6. customthe solvents removed by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-8d979d03afb543558fb79edef7363f43
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08273878B2

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