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Acetic Acid → 5-bromo-7-methylquinazolin-4(3H)-one

HRID 1469759
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반응식

HRID 1469759 반응식
[CH3:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:12])[NH:7][CH:8]=[N:9]2)=[CH:4][CH:3]=1.CO.CC(O)=O.[Br:19]Br>>[Br:19][C:4]1[CH:3]=[C:2]([CH3:1])[CH:11]=[C:10]2[C:5]=1[C:6](=[O:12])[NH:7][CH:8]=[N:9]2
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참가 물질

5

반응물 4

HCID 176Acetic AcidHCID 887MethanolHCID 24408BromineHCID 1354525337-Methyl-4(3H)-quinazolinone

생성물 1

HCID 1363368235-bromo-7-methylquinazolin-4(3H)-one수율 66.9%

실험 절차

To a solution of 7-methylquinazolin-4(3H)-one (900 mg, 5.63 mmol) in MeOH (180 mg, 5.63 mmol) and AcOH (5.07 g, 84.45 mmol) was added bromine (300 μL, 5.63 mmol) and the reaction mixture was stirred at rt for 4 h. Then the reaction mixture was quenched with an aq. solution of sodium thiosulphate. The precipitate obtained was filtered and dried to afford 900 mg of the title product. 1H NMR (300 MHz, DMSO-d6): δ 12.24 (br s, 1H), 8.18 (s, 1H), 8.08 (s, 1H), 7.66 (s, 1H), 2.48 (s, 3H).

후처리

  1. customThen the reaction mixture was quenched with an aq. solution of sodium thiosulphate
  2. customThe precipitate obtained
  3. filtrationwas filtered
  4. customdried

출처 및 근거

ORD 기록
ord-bb17728b65a34f65a65c3a1a9155ae1a
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09006257B2

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