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Glyoxylic Acid → Terbuficin

HRID 436192
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HRID 436192 반응식
[C:1]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:6]=1[OH:15])([CH3:4])([CH3:3])[CH3:2].[C:16]([OH:20])(=[O:19])[CH:17]=O.[OH2:21]>C(Cl)(Cl)(Cl)Cl.Cl>[OH:15][C:6]1[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])=[CH:10][C:9]([CH:17]([C:9]2[CH:10]=[C:5]([C:1]([CH3:3])([CH3:2])[CH3:4])[C:6]([OH:21])=[C:7]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=2)[C:16]([OH:20])=[O:19])=[CH:8][C:7]=1[C:11]([CH3:14])([CH3:13])[CH3:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 760Glyoxylic AcidHCID 962WaterHCID 314052,6-Di-tert-butylphenol

생성물 1

HCID 3084235Terbuficin

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매2회HCID 5943Carbon Tetrachloride용매

반응 조건

온도
50 °C

실험 절차

103 g of 2,6-di-tert.-butyl-phenol (0.5 mol) and 21 g of glyoxylic acid (0.25 mol) of (CHO.COOH) . 1/2 H2O) were dissolved in 300 ml of carbon tetrachloride and stirred at 50° C for about 40 hours. During the first 6 hours, a weak hydrogen chloride stream was passed through the solution, later saturation was completed from time to time by feeding in hydrogen chloride. After condensation was complete, the solvent was eliminated. The product obtained in a pasty form was dissolved and precipitated several times from hexane. The crystallized compound having a faint yellowish tinge melted at 211° C.

후처리

  1. customDuring the first 6 hours
  2. customAfter condensation
  3. customThe product obtained in a pasty form
  4. dissolutionwas dissolved
  5. customprecipitated several times from hexane

출처 및 근거

ORD 기록
ord-34607cfc7e914cb09c42e026741d5972
출처 데이터셋
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04007282

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