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Sulfuric Acid → 3-[7-Methyl-2-oxo-1-(propan-2-yl)-1,2-dihydroquinazolin-4-yl]phenyl acetate

HRID 1834762
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HRID 1834762 반응식
[CH:1]([N:4]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([CH3:14])[CH:12]=2)[C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([OH:21])[CH:16]=2)=[N:6][C:5]1=[O:22])([CH3:3])[CH3:2].S(=O)(=O)(O)O.[C:28](OC(=O)C)(=[O:30])[CH3:29]>>[CH:1]([N:4]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([CH3:14])[CH:12]=2)[C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][C:28](=[O:30])[CH3:29])[CH:16]=2)=[N:6][C:5]1=[O:22])([CH3:3])[CH3:2]
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참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 632573-Hydroxyproquazone

생성물 1

HCID 203719573-[7-Methyl-2-oxo-1-(propan-2-yl)-1,2-dihydroquinazolin-4-yl]phenyl acetate

실험 절차

To 5.0 g of refined 1-isopropyl-4-(3-hydroxyphenyl)-7-methyl-2(1H)-quinazolinone in a vessel, is added 100 ml of acetic anhydride and 0.5 ml. of concentrated sulfuric acid. The resulting mixture is allowed to stand for 16 hours. The reaction mixture is then poured over salted ice in a vessel. After the ice has melted, the resulting liquid is extracted twice with 300 ml portions of benzene: n-butanol (4:1) and the combined extracts washed with distilled water until free of acid, and then evaporated to obtain a residue. The residue is crystallized from methanol to obtain the title product, m.p. 148°-150°.

후처리

  1. additionThe reaction mixture is then poured over salted ice in a vessel
  2. extractionthe resulting liquid is extracted twice with 300 ml portions of benzene: n-butanol (4:1)
  3. washthe combined extracts washed with distilled water until free of acid
  4. customevaporated
  5. customto obtain a residue
  6. customThe residue is crystallized from methanol

출처 및 근거

ORD 기록
ord-3a350b7954194e5a8904abda44d6a736
출처 데이터셋
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04071516

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