Hydrochloric Acid → 2-(7-Chloroquinolin-2-yl)methoxy-11-mercapto-6,11-dihydrodibenz[b,e]oxepine

HRID 232883노트

반응식

HRID 232883 반응식
[OH-].[Na+].C([S:6][CH:7]1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[CH2:11][O:10][C:9]2[CH:18]=[CH:19][C:20]([O:22][CH2:23][C:24]3[CH:33]=[CH:32][C:31]4[C:26](=[CH:27][C:28]([Cl:34])=[CH:29][CH:30]=4)[N:25]=3)=[CH:21][C:8]1=2)(=O)C.O.Cl>C(O)C>[Cl:34][C:28]1[CH:27]=[C:26]2[C:31]([CH:32]=[CH:33][C:24]([CH2:23][O:22][C:20]3[CH:19]=[CH:18][C:9]4[O:10][CH2:11][C:12]5[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=5[CH:7]([SH:6])[C:8]=4[CH:21]=3)=[N:25]2)=[CH:30][CH:29]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 2335910911-Acetylthio-2-(7-chloroquinolin-2-yl)methoxy-6,11-dihydrodibenz[b,e]oxepine

생성물 1

HCID 233591992-(7-Chloroquinolin-2-yl)methoxy-11-mercapto-6,11-dihydrodibenz[b,e]oxepine수율 95.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

19 ml of a 1N-sodium hydroxide aqueous solution was added to 3.49 g of 11-acetylthio-2-(7-chloroquinolin-2-yl)methoxy-6,11-dihydrodibenz[b,e]oxepine obtained in Reference example 71 dissolved in 66 ml of ethanol and the mixture was stirred at room temperature for 1 hour. 250 ml of water was added to the reaction mixture and the mixture was adjusted to about pH 4 with 1N-hydrochloric acid. Crystals precipitated were dissolved in 300 ml of methylene chloride and the organic layer was washed with water and dried over anhydrous sodium sulfate. The solvent was removed to obtain 3.03 g of the title compound as a crude product.

후처리

  1. customobtained in Reference example 71
  2. customCrystals precipitated
  3. dissolutionwere dissolved in 300 ml of methylene chloride
  4. washthe organic layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed

출처 및 근거

ORD 기록
ord-bb938c00b27d4c35ba34ad24a0d63237
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591752

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