Hydrochloric Acid → HCID 13090971, 화합물

HRID 435869노트

반응식

HRID 435869 반응식
[Na].[C:2]([C:5]1[C:26]([OH:27])=[CH:25][CH:24]=[CH:23][C:6]=1[O:7][CH2:8][CH:9]([OH:22])[CH2:10][O:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([OH:18])[C:13]=1[C:19](=[O:21])[CH3:20])(=[O:4])[CH3:3].[C:28](OCC)(=O)[C:29]([O:31][CH2:32][CH3:33])=[O:30].Cl>O.C(Cl)(Cl)Cl.C(O)C>[C:19]([C:13]1[C:14]([OH:18])=[CH:15][CH:16]=[CH:17][C:12]=1[O:11][CH2:10][CH:9]([OH:22])[CH2:8][O:7][C:6]1[C:5]2[C:2](=[O:4])[CH:3]=[C:28]([C:29]([O:31][CH2:32][CH3:33])=[O:30])[O:27][C:26]=2[CH:25]=[CH:24][CH:23]=1)(=[O:21])[CH3:20]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 7268Diethyl OxalateHCID 853031,3-Bis(2-acetyl-3-hydroxyphenoxy) propan-2-olHCID 5360545Sodium

생성물 1

HCID 13090971HCID 13090971, 화합물

시약·촉매·용매 3

HCID 702Ethanol용매2회HCID 962Water용매HCID 6212Chloroform용매

실험 절차

A solution of 69.0 parts of sodium in 1000 parts of ethanol was added to a mixture of 360.3 parts of 1.3 -bis-(2-acetyl-3-hydroxyphenoxy)propan-2-ol, 146.1 parts of diethyl oxalate and 250 parts of ethanol. The reaction mixture was refluxed for five hours, then poured into a stirred mixture of 700 parts of chloroform, 3,000 parts of water and 285 parts of concentrated hydrochloric acid. The solid obtained was removed by filtration, the chloroform phase of the filtrate separated and the aqueous phase extracted with chlroform. The combined chloroform extracts were washed with water and concentrated to give a solid which was removed by filtration. Evaporation of the chloroform from the filtrate give a residue which, after fractional crystallisation from ethanol, gave 36.0 parts of slightly impure ethyl 5-(3-[2-acetyl-3-hydroxyphenoxy]-2-hydroxypropoxy)-4-oxo-4H-1-benzopyran-2-carboxylate, m.pt. 145°-148°.

후처리

  1. temperatureThe reaction mixture was refluxed for five hours
  2. customThe solid obtained
  3. customwas removed by filtration
  4. customthe chloroform phase of the filtrate separated
  5. extractionthe aqueous phase extracted with chlroform
  6. washThe combined chloroform extracts were washed with water
  7. concentrationconcentrated
  8. customto give a solid which
  9. customwas removed by filtration
  10. customEvaporation of the chloroform from the filtrate
  11. customgive a residue which
  12. customafter fractional crystallisation from ethanol

출처 및 근거

ORD 기록
ord-3176fc239bb24b53a2c7aa0ad57cc7d3
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04006245

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