10-Methoxyiminostilbene → 10-methoxy-5H-dibenz(b,f)azepine-5-carboxamide

HRID 2373529

반응식

HRID 2373529 반응식
[CH3:1][O:2][C:3]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[NH:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1.[O-:18][C:19]#[N:20].[Na+].C(O)(=O)/C=C\C(O)=O>ClCCl>[CH3:1][O:2][C:3]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]([C:19]([NH2:20])=[O:18])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=1

참가 물질

5

반응물 3

HCID 7842410-MethoxyiminostilbeneHCID 444266Maleic AcidHCID 517096Sodium Cyanate

생성물 1

HCID 12003110-methoxy-5H-dibenz(b,f)azepine-5-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a 1 L 4-necked round bottom flask was added 10.0 g (0.045 mol) of 10-methoxyiminostilbene, 150.0 ml of dichloromethane, 37.0 g (0.57 mol) of sodium cyanate and 15.0 g (0.13 moles) of maleic acid and stirred at room temperature. The contents were heated to reflux (40-45° C.) under vigorous stirring for about 6 to about 8 hours. After completion of the reaction (detected by TLC) the reaction mass was filtered and washed with 50.0 ml dichloromethane. The dichloromethane layer was washed with water (50.0 ml×2) and the layers were separated.

후처리

  1. temperatureThe contents were heated
  2. temperatureto reflux (40-45° C.)
  3. stirringunder vigorous stirring for about 6 to about 8 hours
  4. customAfter completion of the reaction (detected by TLC) the reaction mass
  5. filtrationwas filtered
  6. washwashed with 50.0 ml dichloromethane
  7. washThe dichloromethane layer was washed with water (50.0 ml×2)
  8. customthe layers were separated

출처 및 근거

ORD 기록
ord-85a333037c23477695f1d21a68f04e93
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07459553B2

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