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Water → 2-Acetylamino-4-allylamino-6-nitroquinazoline

HRID 1250595
ノート
印刷プレビュー

反応式

HRID 1250595 の反応式
[CH2:1]([NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([N+:15]([O-:17])=[O:16])[CH:13]=2)[N:8]=[C:7]([NH2:18])[N:6]=1)[CH:2]=[CH2:3].[C:19](OC(=O)C)(=[O:21])[CH3:20].C(N(CC)CC)C.O>C(#N)C>[C:19]([NH:18][C:7]1[N:6]=[C:5]([NH:4][CH2:1][CH:2]=[CH2:3])[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([N+:15]([O-:17])=[O:16])[CH:13]=2)[N:8]=1)(=[O:21])[CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 183264494-Allylamino-2-amino-6-nitroquinazoline

生成物 1

HCID 183264972-Acetylamino-4-allylamino-6-nitroquinazoline収率 80.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

After 100 mg (0.41 mmol) of 4-allylamino-2-amino-6-nitroquinazoline was dissolved in 10 ml of acetonitrile, 84 mg (0.82 mmol) of acetic anhydride and 0.06 ml (0.45 mmol) of triethylamine were added thereto, and then the reaction mixture was subjected to heating under reflux overnight. Water was added to the reaction solution, followed by extraction with ethyl acetate, washing successively with a saturated aqueous sodium hydrogen carbonate solution and brine and drying over anhydrous sodium sulfate. The solvent was distilled off, followed by recrystallization from ethyl acetate-hexane to give 95 mg (80.7%) of the title compound.

後処理

  1. temperatureto heating
  2. temperatureunder reflux overnight
  3. extractionfollowed by extraction with ethyl acetate
  4. washwashing successively with a saturated aqueous sodium hydrogen carbonate solution and brine
  5. dry with materialdrying over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off
  7. customfollowed by recrystallization from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-7e07d75a983747129548e60364d33475
出典データセット
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06339089B2

反応ノート

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