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1,3-Dichloroacetone → 2-(Chloromethyl)-5,7-dimethylimidazo[1,2-a]pyrimidine

HRID 537889
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HRID 537889 반응식
[NH2:1][C:2]1[N:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[N:3]=1.[Cl:10][CH2:11][C:12](=O)[CH2:13]Cl>COCCOC>[Cl:10][CH2:11][C:12]1[N:1]=[C:2]2[N:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[N:3]2[CH:13]=1
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참가 물질

4

반응물 2

HCID 107931,3-DichloroacetoneHCID 130212-Amino-4,6-dimethyl pyrimidine

생성물 1

HCID 6933302-(Chloromethyl)-5,7-dimethylimidazo[1,2-a]pyrimidine

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

A solution of 2-amino-4,6-dimethylpyrimidine (2.46 g, 20.0 mmol) and 1,3-dichloro-2-propanone (2.67 g, 21.0 mmol) in 1,2-dimethoxyethane (20 mL) was stirred at 45° C. overnight. A precipitate formed, and this was collected by filtration, and was then refluxed with ethanol (15 mL) for 2 hours. After cooling to room temperature, the product precipitated as white needles which were collected by filtration and vacuum dried to yield the title compound pure as its hydrochloride salt (883 mg, 19%). 1H NMR (500 MHz, DMSO-d6): δ7.84 (s, 1H), 6.88 (s, 1H), 4.84 (s, 2H), 2.60 (s, 3H), 2.49 (s, 3H).

후처리

  1. customA precipitate formed
  2. filtrationthis was collected by filtration
  3. temperaturewas then refluxed with ethanol (15 mL) for 2 hours
  4. customthe product precipitated as white needles which
  5. filtrationwere collected by filtration and vacuum
  6. customdried

출처 및 근거

ORD 기록
ord-29ded83cce7145df887ef8f67432a690
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08865711B2

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