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Hydrochloric Acid → Methyl(4-(4-bromobenzylamino)-2,6-dimethylpyrimidin-5-yl)ketone

HRID 129019
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인쇄 미리보기

반응식

HRID 129019 반응식
[Br:1][C:2]1[CH:22]=[CH:21][C:5]([CH2:6][NH:7][C:8]2[C:13]([C:14]([O:16]CC)=[CH2:15])=[C:12]([CH3:19])[N:11]=[C:10]([CH3:20])[N:9]=2)=[CH:4][CH:3]=1.Cl>CC(C)=O>[CH3:15][C:14]([C:13]1[C:8]([NH:7][CH2:6][C:5]2[CH:4]=[CH:3][C:2]([Br:1])=[CH:22][CH:21]=2)=[N:9][C:10]([CH3:20])=[N:11][C:12]=1[CH3:19])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 107373314-(4-Bromobenzylamino)-2,6-dimethyl-5-(1-ethoxyvinyl)pyrimidine

생성물 1

HCID 10688121Methyl(4-(4-bromobenzylamino)-2,6-dimethylpyrimidin-5-yl)ketone수율 89.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A solution of 4-(4-bromobenzylamino)-2,6-dimethyl-5-(1-ethoxyvinyl)pyrimidine (2.72 g, 7.51 mmol), 1N HCl (8.3 mL), and acetone (8 mL) was heated under reflux for 2.5 h. The acetone was removed under reduced pressure and the aqueous phase was adjusted to pH 4 with 1N KOH. The resultant white precipitate was collected by filtration to give 2.24 g (89%) of product as a white solid. An analytical sample was recrystallized from hexane, mp 78°-80° C.

후처리

  1. temperatureunder reflux for 2.5 h
  2. customThe acetone was removed under reduced pressure
  3. filtrationThe resultant white precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-a831f563ccab4f2f8b953310d6677e38
출처 데이터셋
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05466692

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