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

HRID 232883ノート

反応式

HRID 232883 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bb938c00b27d4c35ba34ad24a0d63237
出典データセット
uspto-grants-1997_01
特許番号
US05591752

反応ノート

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