Hydrochloric Acid → HCID 13090971、化合物

HRID 435869ノート

反応式

HRID 435869 の反応式
[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]

参加物

8

反応物 4

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

生成物 1

HCID 13090971HCID 13090971、化合物

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒2 回HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-3176fc239bb24b53a2c7aa0ad57cc7d3
出典データセット
uspto-grants-1977_02
特許番号
US04006245

反応ノート

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