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

HRID 1834762
ノート
印刷プレビュー

反応式

HRID 1834762 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 632573-Hydroxyproquazone

生成物 1

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

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-3a350b7954194e5a8904abda44d6a736
出典データセット
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04071516

反応ノート

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