Piperidine → HCID 17789091, 화합물

HRID 747669

반응식

HRID 747669 반응식
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl-].[C:8](OC)(=[O:18])[C:9]1[CH:17]=[CH:16][C:12]([C:13]([O-:15])=[O:14])=[CH:11][CH:10]=1>ClCCl.Cl>[N:1]1([C:8]([C:9]2[CH:17]=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[CH:11][CH:10]=2)=[O:18])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 8082PiperidineHCID 22493623Monomethyl terephthalate chloride

생성물 1

HCID 17789091HCID 17789091, 화합물

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 6344Dichloromethane용매2회

실험 절차

6 ml of piperidine was stirred in dichloromethane at 0° C., and a solution of 3 g (15 mmol) of monomethyl terephthalate chloride in dichloromethane was added to the resultant mixture. The temperature was elevated to room temperature, and they were stirred for 2 hours and then diluted with 1 N hydrochloric acid. After the extraction with dichloromethane, the organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and then with saturated aqueous NaCl solution, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was stirred in ethanol. 30 ml of 1 N aqueous sodium hydroxide solution was added to the resultant mixture, and they were stirred at room temperature overnight. The solvent was evaporated, and the reaction liquid was concentrated and then diluted with 1 N hydrochloric acid. After the extraction with ethyl acetate, the organic layer was washed with saturated aqueous NaCl solution and dried over anhydrous magnesium sulfate. The solvent was evaporated to obtain the title compound.

후처리

  1. customwas elevated to room temperature
  2. extractionAfter the extraction with dichloromethane
  3. washthe organic layer was washed with saturated aqueous sodium hydrogencarbonate solution
  4. dry with materialwith saturated aqueous NaCl solution, and dried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated
  6. stirringthe residue was stirred in ethanol
  7. addition30 ml of 1 N aqueous sodium hydroxide solution was added to the resultant mixture, and they
  8. stirringwere stirred at room temperature overnight
  9. customThe solvent was evaporated
  10. customthe reaction liquid
  11. concentrationwas concentrated
  12. additiondiluted with 1 N hydrochloric acid
  13. extractionAfter the extraction with ethyl acetate
  14. washthe organic layer was washed with saturated aqueous NaCl solution
  15. dry with materialdried over anhydrous magnesium sulfate
  16. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-c5224bb818f548b19fd2ebc46b44c197
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07396844B1

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