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Sodium Bicarbonate → 1-Amino-6,11-dihydrodibenz[b,e]oxepin-11-one

HRID 1827
ノート
印刷プレビュー

反応式

HRID 1827 の反応式
C([NH:4][C:5]1[C:15]2[C:14](=[O:16])[C:13]3[CH:17]=[CH:18][CH:19]=[CH:20][C:12]=3[CH2:11][O:10][C:9]=2[CH:8]=[CH:7][CH:6]=1)(=O)C.C(=O)(O)[O-].[Na+]>Cl>[NH2:4][C:5]1[C:15]2[C:14](=[O:16])[C:13]3[CH:17]=[CH:18][CH:19]=[CH:20][C:12]=3[CH2:11][O:10][C:9]=2[CH:8]=[CH:7][CH:6]=1
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 516892Sodium BicarbonateHCID 196930381-Acetamido-6,11-dihydrodibenz[b,e]oxepin-11-one

生成物 1

HCID 196930241-Amino-6,11-dihydrodibenz[b,e]oxepin-11-one収率 81%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

In concentrated hydrochloric acid (10 ml), 1-acetamido-6,11-dihydrodibenz[b,e]oxepin-11-one obtained in Reference Example 3(0.25 g, 0.94 mmol) was heated under reflux for 2 hours. The reaction mixture was poured into a saturated aqueous solution of sodium bicarbonate, followed by extraction with ethyl acetate (25 ml). The organic layer was washed with a saturated aqueous solution of sodium chloride, and then dried over anhydrous magnesium sulfate. After the drying agent was filtered off, the organic layer was concentrated under reduced pressure to give 1-amino-6,11-dihydrodibenz[b,e]oxepin-11-one as a yellow solid (0.17 g, 81%).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. extractionfollowed by extraction with ethyl acetate (25 ml)
  4. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationAfter the drying agent was filtered off
  7. concentrationthe organic layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-cca8c52f7ba34625b95aa6d245498aa5
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05726325

反応ノート

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