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

HRID 41347
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HRID 41347 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(C1C=CC=CC=1)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 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1292Mandelic AcidHCID 7842410-MethoxyiminostilbeneHCID 517096Sodium Cyanate

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A suspension of 10 g of 10-methoxyiminostilbene in 250 ml dichloromethane was treated with 17.5 g of sodium cyanate and 24 g of mandelic acid and was heated to reflux for about 6-8 hrs. The reaction mixture was cooled to room temperature and the reaction mixture was washed with distilled water and aqueous sodium bicarbonate and further the organic layer was distilled off completely. The resulting residue was treated with isopropanol; separated solid was filtered and dried to give 10-methoxy carbamazepine.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for about 6-8 hrs
  3. washthe reaction mixture was washed with distilled water and aqueous sodium bicarbonate
  4. distillationfurther the organic layer was distilled off completely
  5. additionThe resulting residue was treated with isopropanol
  6. customseparated solid
  7. filtrationwas filtered
  8. customdried

출처 및 근거

ORD 기록
ord-58bd4edf32fb443ea85d510b7142241e
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08530647B2

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