Hydrochloric Acid → Oxane-4-carboxylic acid

HRID 2104368노트

반응식

HRID 2104368 반응식
C[O:2][C:3]([C:5]1(C(OC)=O)[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1)=[O:4].Cl>O>[O:8]1[CH2:9][CH2:10][CH:5]([C:3]([OH:4])=[O:2])[CH2:6][CH2:7]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 11063483Dimethyl Tetrahydropyran-4,4-dicarboxylate

생성물 1

HCID 219302Oxane-4-carboxylic acid수율 101.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To tetrahydro-4H-pyran-4,4-dicarboxylic acid dimethyl ester (4.04 g) was added 20% HCl (20 mL), and the mixture was heated under reflux for 19 hours. Water was added to the reaction mixture, and the thus-obtained mixture was extracted with diethyl ether. The organic layer was washed with saturated brine, and was dried over sodium sulfate anhydrate. The solvent was distilled away under reduced pressure, and hexane was added to the residue. The resultant solid was collected by filtration, and was washed, to thereby give the title compound (2.63 g).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 19 hours
  3. extractionthe thus-obtained mixture was extracted with diethyl ether
  4. washThe organic layer was washed with saturated brine
  5. dry with materialwas dried over sodium sulfate anhydrate
  6. distillationThe solvent was distilled away under reduced pressure, and hexane
  7. additionwas added to the residue
  8. filtrationThe resultant solid was collected by filtration
  9. washwas washed

출처 및 근거

ORD 기록
ord-3c08847dfb9f441b85721b45d9db14e9
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576135B2

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