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Ethanol → HCID 13079788, 화합물

HRID 1284089
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HRID 1284089 반응식
Cl[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:7][CH:6]=1)=O.C(O)C.[NH2:20][C:21]1[N:26]=[CH:25][CH:24]=[CH:23][N:22]=1>C1C=CC=CC=1>[N:20]1[C:3]([C:5]2[CH:10]=[CH:9][C:8]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:7][CH:6]=2)=[CH:2][N:22]2[CH:23]=[CH:24][CH:25]=[N:26][C:21]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 79782-AminopyrimidineHCID 12399236HCID 12399236, 화합물

생성물 1

HCID 13079788HCID 13079788, 화합물수율 46.3%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture of 48 g of ethyl 4-(chloroacetyl)phenylacetate, 100 ml of ethanol and 38 g of 2-aminopyrimidine is heated under reflux for 3 hours. The ethanol is distilled off under reduced pressure, and water is added to the residue. The mixture is extracted with ethyl acetate, and the extract is washed with water, dried and concentrated to give a brown oil. To the oil is added benzene, and the crystalline precipitate is filtered off and recrystallized from ethyl acetate to give 26 g of ethyl 4-(imidazo[1,2-a]-pyrimidine-2-yl)phenylacetate as pale brown crystals melting at 155°-158°C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 3 hours
  3. distillationThe ethanol is distilled off under reduced pressure, and water
  4. additionis added to the residue
  5. extractionThe mixture is extracted with ethyl acetate
  6. washthe extract is washed with water
  7. customdried
  8. concentrationconcentrated
  9. customto give a brown oil
  10. filtrationthe crystalline precipitate is filtered off
  11. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-e190c8ea8dea477bb72a0551ba2b2060
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03978071

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