Toluene → 3-(3,5-Di-t-butyl-4-hydroxyphenyl)-propionic acid allyl ester

HRID 2059123

반응식

HRID 2059123 반응식
[NH2-].[Li+].[CH2:3]([OH:6])[CH:4]=[CH2:5].C[O:8][C:9](=O)[CH2:10][CH2:11][C:12]1[CH:17]=[C:16]([C:18]([CH3:21])([CH3:20])[CH3:19])[C:15]([OH:22])=[C:14]([C:23]([CH3:26])([CH3:25])[CH3:24])[CH:13]=1.C1(C)C=CC=CC=1>C(O)(=O)C>[CH2:3]([O:6][C:9](=[O:8])[CH2:10][CH2:11][C:12]1[CH:17]=[C:16]([C:18]([CH3:19])([CH3:21])[CH3:20])[C:15]([OH:22])=[C:14]([C:23]([CH3:26])([CH3:25])[CH3:24])[CH:13]=1)[CH:4]=[CH2:5]

참가 물질

6

반응물 4

HCID 1140TolueneHCID 7858Allyl AlcoholHCID 24532Lithium amideHCID 62603Methyl di-t-butyl hydroxyhydrocinnamate

생성물 1

HCID 205457203-(3,5-Di-t-butyl-4-hydroxyphenyl)-propionic acid allyl ester

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
150 °C

실험 절차

0.2 g of lithium amide and in the course of 5 hours 38 g of allyl alcohol are added at 150° C. under nitrogen to 146 g of 3-(3,5-di-t-butyl-4-hydroxyphenyl)-propionic acid methyl ester. After completion of the addition, stirring is maintained at 150° C. for a further 10 hours. The brownish reaction mixture is cooled to about 100° C., and 150 ml of toluene, 0.5 g of concentrated acetic acid and 10 g of "Celite Hyflow Supercel" (product of Johns Manville Corp., USA) are added. There is thus obtained, after filtration and then removal of the solvent in vacuo, the title compound in crystalline form, m.p. about 40° C.

후처리

  1. additionAfter completion of the addition
  2. customThe brownish reaction mixture
  3. temperatureis cooled to about 100° C.
  4. customThere is thus obtained
  5. filtrationafter filtration
  6. customremoval of the solvent in vacuo

출처 및 근거

ORD 기록
ord-504d49677280405fba3127a71044c487
출처 데이터셋
uspto-grants-1982_03
특허 번호
US04322303

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