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

HRID 1827
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HRID 1827 반응식
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
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참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 196930381-Acetamido-6,11-dihydrodibenz[b,e]oxepin-11-one

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-cca8c52f7ba34625b95aa6d245498aa5
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05726325

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