Potassium Carbonate → 2-(7-Chloroquinolin-2-yl)methoxy-11-(3-ethoxycarbonylpropylthio)-6,11-dihydrodibenz[b,e]oxepine

HRID 232847ノート

反応式

HRID 232847 の反応式
C(=O)([O-])[O-].[K+].[K+].[Cl:7][C:8]1[CH:17]=[C:16]2[C:11]([CH:12]=[CH:13][C:14]([CH2:18][O:19][C:20]3[CH:35]=[CH:34][C:23]4[O:24][CH2:25][C:26]5[CH:33]=[CH:32][CH:31]=[CH:30][C:27]=5[CH:28]([SH:29])[C:22]=4[CH:21]=3)=[N:15]2)=[CH:10][CH:9]=1.Br[CH2:37][CH2:38][CH2:39][C:40]([O:42][CH2:43][CH3:44])=[O:41]>CC(C)=O>[Cl:7][C:8]1[CH:17]=[C:16]2[C:11]([CH:12]=[CH:13][C:14]([CH2:18][O:19][C:20]3[CH:35]=[CH:34][C:23]4[O:24][CH2:25][C:26]5[CH:33]=[CH:32][CH:31]=[CH:30][C:27]=5[CH:28]([S:29][CH2:37][CH2:38][CH2:39][C:40]([O:42][CH2:43][CH3:44])=[O:41])[C:22]=4[CH:21]=3)=[N:15]2)=[CH:10][CH:9]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 76300Ethyl 4-bromobutyrateHCID 233591992-(7-Chloroquinolin-2-yl)methoxy-11-mercapto-6,11-dihydrodibenz[b,e]oxepine

生成物 1

HCID 233591262-(7-Chloroquinolin-2-yl)methoxy-11-(3-ethoxycarbonylpropylthio)-6,11-dihydrodibenz[b,e]oxepine収率 67.6%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

0.43 g of potassium carbonate was added to 1 g of 2-(7-chloroquinolin-2-yl)methoxy-11-mercapto-6,11-dihydrodibenz[b,e]oxepine and 0.56 g of ethyl 4-bromobutanoate dissolved in 25 ml of acetone and the mixture was stirred under heating for 3 hours. After completion of the reaction, the reaction mixture was filtered and the filtrate was condensed under reduced pressure. The resulting residue was applied to silica gel column chromatography to obtain 0.86 g of 2-(7-chloroquinolin-2-yl)methoxy-11-(3-ethoxycarbonylpropylthio)-6,11-dihydrodibenz[b,e]oxepine as a brown oily product.

後処理

  1. temperatureunder heating for 3 hours
  2. customAfter completion of the reaction
  3. filtrationthe reaction mixture was filtered
  4. customcondensed under reduced pressure

出典と根拠

ORDレコード
ord-cee62b149fc849b294935b46a407723b
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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