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Hydrochloric Acid → (7-(4-(4-(Benzo[b]thiophen-4-yl)piperazin-1-yl)butoxy)-2-oxoquinolin-1(2h)-yl)methyl cyclohexyl carbonate hydrochloride

HRID 1774698
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HRID 1774698 반응식
[H-].[Na+].[S:3]1[CH:7]=[CH:6][C:5]2[C:8]([N:12]3[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][CH2:20][CH2:21][O:22][C:23]4[CH:32]=[C:31]5[C:26]([CH:27]=[CH:28][C:29](=[O:33])[NH:30]5)=[CH:25][CH:24]=4)[CH2:14][CH2:13]3)=[CH:9][CH:10]=[CH:11][C:4]1=2.[C:34](=[O:45])([O:38][CH:39]1[CH2:44][CH2:43][CH2:42][CH2:41][CH2:40]1)[O:35][CH2:36][Cl:37].Cl>O1CCCC1>[ClH:37].[CH:39]1([O:38][C:34](=[O:45])[O:35][CH2:36][N:30]2[C:31]3[C:26](=[CH:25][CH:24]=[C:23]([O:22][CH2:21][CH2:20][CH2:19][CH2:18][N:15]4[CH2:14][CH2:13][N:12]([C:8]5[C:5]6[CH:6]=[CH:7][S:3][C:4]=6[CH:11]=[CH:10][CH:9]=5)[CH2:17][CH2:16]4)[CH:32]=3)[CH:27]=[CH:28][C:29]2=[O:33])[CH2:44][CH2:43][CH2:42][CH2:41][CH2:40]1
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 11978813BrexpiprazoleHCID 13603586Chloromethyl cyclohexyl carbonate

생성물 1

HCID 117855958(7-(4-(4-(Benzo[b]thiophen-4-yl)piperazin-1-yl)butoxy)-2-oxoquinolin-1(2h)-yl)methyl cyclohexyl carbonate hydrochloride수율 42%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

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온도
50 °C

실험 절차

Sodium hydride (55% oil) (0.962 g, 22.04 mmol) was suspended in tetrahydrofuran (THF) (200 ml), 7-[4-(4-benzo[b]thiophen-4-yl-piperazin-1-yl)-butoxy]-1H-quinolin-2-one (8.31 g, 19.17 mmol) was added and the mixture was stirred at 50° C. for 1 hr. The mixture was cooled to 0° C., chloromethyl cyclohexyl carbonate (4.80 g, 24.92 mmol) was added dropwise and the mixture was stirred at room temperature overnight. After cooling to 0° C., excess 2N hydrochloric acid was added to quench the reaction. The precipitated solid was collected by filtration and dried. In addition, the filtrate was extracted with ethyl acetate. The organic layer was concentrated and purified by moderate-pressure silica gel column chromatography (methylene chloride:methanol=100:0 to 20:1). Likewise, the solid was purified by moderate-pressure silica gel column chromatography. Concentration under reduced pressure gave the title compound (yield, 5.04 g, 42%) as a white solid.

후처리

  1. temperatureThe mixture was cooled to 0° C.
  2. stirringthe mixture was stirred at room temperature overnight
  3. temperatureAfter cooling to 0° C.
  4. customto quench
  5. customthe reaction
  6. filtrationThe precipitated solid was collected by filtration
  7. customdried
  8. extractionIn addition, the filtrate was extracted with ethyl acetate
  9. concentrationThe organic layer was concentrated
  10. custompurified by moderate-pressure silica gel column chromatography (methylene chloride:methanol=100:0 to 20:1)
  11. customLikewise, the solid was purified by moderate-pressure silica gel column chromatography
  12. concentrationConcentration under reduced pressure

출처 및 근거

ORD 기록
ord-ec45c34668f340228b41cb252d8c7ee2
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09260420B2

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