Acetic Acid → 2-(7-Chloro-6-fluoroquinolin-2-yl)methoxy-11-hydroxy-8-(2-acetylethyl)-6,11-dihydrodibenz[b,e]oxepine

HRID 232885

반응식

HRID 232885 반응식
FC(F)(F)C(O)=O.[Cl:8][C:9]1[CH:18]=[C:17]2[C:12]([CH:13]=[CH:14][C:15]([CH2:19][O:20][C:21]3[CH:47]=[CH:46][C:24]4[O:25][CH2:26][C:27]5[CH:40]=[C:39]([CH2:41][CH2:42][C:43](=[O:45])[CH3:44])[CH:38]=[CH:37][C:28]=5[CH:29]([O:30]C5CCCCO5)[C:23]=4[CH:22]=3)=[N:16]2)=[CH:11][C:10]=1[F:48].C(O)(=O)C>O1CCOCC1.O>[Cl:8][C:9]1[CH:18]=[C:17]2[C:12]([CH:13]=[CH:14][C:15]([CH2:19][O:20][C:21]3[CH:47]=[CH:46][C:24]4[O:25][CH2:26][C:27]5[CH:40]=[C:39]([CH2:41][CH2:42][C:43](=[O:45])[CH3:44])[CH:38]=[CH:37][C:28]=5[CH:29]([OH:30])[C:23]=4[CH:22]=3)=[N:16]2)=[CH:11][C:10]=1[F:48]

참가 물질

6

실험 절차

0.02 ml of trifluoroacetic acid was added to 0.73 g of 2-(7-chloro-6-fluoroquinolin-2-yl)methoxy-8-(2-acetylethyl)-11-(2-tetrahydropyranyloxy)-6,11-dihydrodibenz[b,e]oxepine obtained in Reference example 74 dissolved in a mixed solution of 5 ml of dioxane and 2 ml of water, the mixture was stirred at room temperature for 15 minutes, 4 ml of acetic acid was added to the mixture and the mixture was stirred for 10 hours. 80 ml of water was added to the reaction mixture and insolubles were removed by filtration. The residue was dissolved in chloroform and the organic layer was washed with water and dried over anhydrous sodium sulfate. After the solvent was removed, the residue was washed with a mixed solution of acetone and ether to obtain 0.41 g of the title compound.

후처리

  1. customobtained in Reference example 74
  2. stirringthe mixture was stirred for 10 hours
  3. customwere removed by filtration
  4. dissolutionThe residue was dissolved in chloroform
  5. washthe organic layer was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customAfter the solvent was removed
  8. washthe residue was washed with a mixed solution of acetone and ether

출처 및 근거

ORD 기록
ord-ba4536a181754e39a127951667b20ab4
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591752

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