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

HRID 1982372
ノート
印刷プレビュー

反応式

HRID 1982372 の反応式
[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17](Cl)=[O:18])=[CH:16][C:3]1=2.[NH3:20]>O1CCCC1>[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17]([NH2:20])=[O:18])=[CH:16][C:3]1=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 2

HCID 222AmmoniaHCID 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

実験手順

The remaining half of the acid chloride IV was added to a mixture of 150 ml of concentrated ammonia and 150 ml of tetrahydrofuran. Then, the mixture was stirred at room temperature for three hours and concentrated under reduced pressure. The residue was vigorously stirred together with 300 ml of saturated aqueous solution of sodium bicarbonate and 100 ml of ether, and the solid was collected by filtration and dried to obtain 6,11-dihydro-11-oxodibenz[b,e]oxepin-2-carboamide VIII in a quantitative yield. Recrystallization from methanol gave pure crystals having a melting point of 227°-228° C. IR spectrum (KBr tablet, cm-1): 3430, 3150, 1680, 1635, 1600, 1370.

後処理

  1. concentrationconcentrated under reduced pressure
  2. stirringThe residue was vigorously stirred together with 300 ml of saturated aqueous solution of sodium bicarbonate and 100 ml of ether
  3. filtrationthe solid was collected by filtration
  4. customdried

出典と根拠

ORDレコード
ord-964c45345b2b4a7296b2a45afb0ef1fa
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04596804

反応ノート

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