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Hydrochloric Acid → 2-Chloro-3-pyridinecarboxaldehyde

HRID 55519
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HRID 55519 반응식
CCCCCC.[H-].C([Al+]CC(C)C)C(C)C.[Cl:17][C:18]1[C:23]([C:24]#N)=[CH:22][CH:21]=[CH:20][N:19]=1.Cl.[O:27]1CCCC1>>[Cl:17][C:18]1[C:23]([CH:24]=[O:27])=[CH:22][CH:21]=[CH:20][N:19]=1
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참가 물질

6

반응물 5

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 8058HexaneHCID 810792-ChloronicotinonitrileHCID 21225700Diisobutylaluminumhydride

생성물 1

HCID 7376072-Chloro-3-pyridinecarboxaldehyde

실험 절차

200 ml of a 1.02M hexane solution of diisobutylaluminum hydride were added to a solution of 16.7 g of 2-chloro-3-cyanopyridine in 200 ml of tetrahydrofuran at a temperature of -30° to 20° C. over a period of 30 minutes, after which the resulting mixture was stirred at room temperature for 1 hour. At the end of this time, hydrochloric acid was added to the reaction mixture at 0° C, and then the mixture was extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium carbonate and with a saturated aqueous solution of sodium chloride, in that order, and then dried over anhydrous sodium sulfate, after which the solvent was removed by distillation under reduced pressure. The residue was purified by column chromatography through silica gel, using a gradient elution method, with mixtures of hexane and ethyl acetate in ratios ranging from 6:1 to 5:1 by volume as the eluent, to give 7.0 g of the title compound having Rf=0.50 (on silica gel thin layer chromatography using a 2:1 by volume mixture of hexane and ethyl acetate as the developing solvent).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with a saturated aqueous solution of sodium carbonate and with a saturated aqueous solution of sodium chloride, in that order
  3. dry with materialdried over anhydrous sodium sulfate
  4. customafter which the solvent was removed by distillation under reduced pressure
  5. customThe residue was purified by column chromatography through silica gel
  6. washa gradient elution method

출처 및 근거

ORD 기록
ord-bca1c7e2895a405dbcd1e40db5c70359
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05624935

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