Ammonia → 6,11-Dihydro-11-oxodibenz[b,e]oxepin-2-carboamide

HRID 894193ノート

反応式

HRID 894193 の反応式
Cl[C:2]([C:4]1[CH:19]=[CH:18][C:7]2[O:8][CH2:9][C:10]3[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=3[C:12](=[O:13])[C:6]=2[CH:5]=1)=[O:3].[NH3:20]>O1CCCC1>[O:13]=[C:12]1[C:11]2[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=2[CH2:9][O:8][C:7]2[CH:18]=[CH:19][C:4]([C:2]([NH2:20])=[O:3])=[CH:5][C:6]1=2

参加物

4

反応物 2

HCID 222Ammonia2 回HCID 134560052-Chlorocarbonyl-6,11-dihydro-11-oxodibenz[b,e]oxepin

生成物 1

HCID 124468236,11-Dihydro-11-oxodibenz[b,e]oxepin-2-carboamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Dissolve the acid chloride from Step A in 20 ml. of dry tetrahydrofuran and add this solution dropwise with stirring to a cooled (ice-bath) saturated solution of ammonia in 60 ml. of tetrahydrofuran. Pass ammonia through the reaction mixture simultaneously for 15 minutes. Stir at room temperature for an additional 15 minutes and evaporate the reaction mixture to dryness. Add a mixture of 12 ml. of ethanol and 60 ml. of water to the residue and stir at room temperature for an additional 30 minutes. Separate the solid by filtration and wash with water, then with ethanol and then with ether. Dry in vacuo to obtain the title product.

後処理

  1. stirringStir at room temperature for an additional 15 minutes
  2. customevaporate the reaction mixture to dryness
  3. additionAdd
  4. additiona mixture of 12 ml
  5. stirringof water to the residue and stir at room temperature for an additional 30 minutes
  6. customSeparate the solid
  7. filtrationby filtration
  8. washwash with water
  9. customDry in vacuo

出典と根拠

ORDレコード
ord-273c4663703e4349988802136b904ff6
出典データセット
uspto-grants-1981_08
特許番号
US04282365

反応ノート

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