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Water → 7-Benzyloxy-6-cyano-4-(1H-indol-5-yloxy)quinoline

HRID 387873
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HRID 387873 반응식
[CH2:1]([O:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13](Cl)=[CH:14][CH:15]=[N:16]2)=[CH:11][C:10]=1[C:20]#[N:21])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH:22][C:23]1[CH:24]=[C:25]2[C:29](=[CH:30][CH:31]=1)[NH:28][CH:27]=[CH:26]2.C(N(C(C)C)CC)(C)C.O>CN1CCCC1=O.O1CCCC1>[CH2:1]([O:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13]([O:22][C:23]3[CH:24]=[C:25]4[C:29](=[CH:30][CH:31]=3)[NH:28][CH:27]=[CH:26]4)=[CH:14][CH:15]=[N:16]2)=[CH:11][C:10]=1[C:20]#[N:21])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

7

반응물 4

HCID 962WaterHCID 160545-HydroxyindoleHCID 81531DiisopropylethylamineHCID 226465197-Benzyloxy-4-chloro-6-cyanoquinoline

생성물 1

HCID 229364817-Benzyloxy-6-cyano-4-(1H-indol-5-yloxy)quinoline수율 40.92%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran
용매
HCID 13387N-methyl-2-pyrrolidone용매

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온도
150 °C

실험 절차

After suspending 7-benzyloxy-6-cyano-4-chloroquinoline (23 g, 78.03 mmol) in N-methylpyrrolidone (15.8 ml), there were added 5-hydroxyindole (12.5 g, 83.64 mmol) and diisopropylethylamine (15.8 ml) and the mixture was heated and stirred at 150° C. for 10 hours. After allowing it to cool to room temperature, water and tetrahydrofuran were added and the crystals were thoroughly dissolved. After extraction with tetrahydrofuran, washing with saturated saline, drying over anhydrous magnesium sulfate and distilling off of the solvent, the residue was adsorbed onto silica gel. Purification was performed by silica gel column chromatography (hexane/tetrahydrofuran system), and then concentrated hydrochloric acid (0.2 ml) was added at room temperature and the mixture was stirred for 17 hours. The solvent was distilled off under reduced pressure, saturated bicarbonate water was added, and then extraction was performed with a tetrahydrofuran and ethyl acetate mixed solvent, the extract was washed with saturated saline and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The obtained crystals were suspended in ethyl acetate and diluted with diethyl ether and hexane. The crystals were filtered out, washed with diethyl ether/hexane and dried by aspiration to obtain the title compound (12.5 g, 31.93 mmol, 40.92%) as light yellow crystals.

후처리

  1. temperaturethe mixture was heated
  2. temperatureto cool to room temperature
  3. dissolutionthe crystals were thoroughly dissolved
  4. extractionAfter extraction with tetrahydrofuran
  5. washwashing with saturated saline
  6. dry with materialdrying over anhydrous magnesium sulfate
  7. distillationdistilling off of the solvent
  8. customPurification
  9. additionconcentrated hydrochloric acid (0.2 ml) was added at room temperature
  10. stirringthe mixture was stirred for 17 hours
  11. distillationThe solvent was distilled off under reduced pressure, saturated bicarbonate water
  12. additionwas added
  13. extractionextraction
  14. washthe extract was washed with saturated saline
  15. dry with materialdried over anhydrous magnesium sulfate
  16. distillationthe solvent was distilled off under reduced pressure
  17. additiondiluted with diethyl ether and hexane
  18. filtrationThe crystals were filtered out
  19. washwashed with diethyl ether/hexane
  20. customdried by aspiration

출처 및 근거

ORD 기록
ord-3cd65e45d05141abaa0bc2ed6cd01ddd
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08372981B2

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