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

HRID 232847노트

반응식

HRID 232847 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-cee62b149fc849b294935b46a407723b
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591752

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