Hydrochloric Acid → HCID 13090971, 화합물

HRID 2163403노트

반응식

HRID 2163403 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 chloroform. 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 gave a residue which, after fractional crystallization 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 chloroform
  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. customgave a residue which
  12. customafter fractional crystallization from ethanol

출처 및 근거

ORD 기록
ord-8ad5e0b04df04feea61959230fc434f8
출처 데이터셋
uspto-grants-1979_01
특허 번호
US04133889

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