2,4-Dimethylphenol → 2-Hydroxy-3,5-dimethyl phenyl-p-diisopropyl benzene

HRID 1764440

반응식

HRID 1764440 반응식
O[C:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11](O)([CH3:13])[CH3:12])=[CH:7][CH:6]=1)([CH3:4])[CH3:3].[CH3:15][C:16]1[CH:21]=[C:20]([CH3:22])[CH:19]=[CH:18][C:17]=1[OH:23]>>[OH:23][C:17]1[C:16]([CH3:15])=[CH:21][C:20]([CH3:22])=[CH:19][C:18]=1[C:9]1[CH:10]=[C:5]([CH:2]([CH3:4])[CH3:3])[CH:6]=[CH:7][C:8]=1[CH:11]([CH3:13])[CH3:12]

참가 물질

3

반응물 2

HCID 77712,4-Dimethylphenol2회HCID 18062p-Bis(2-hydroxyisopropyl)benzene

생성물 1

HCID 867360332-Hydroxy-3,5-dimethyl phenyl-p-diisopropyl benzene수율 80%

실험 절차

A solution of 1164 g (6 mols) of α,α'-dihydroxy-p-diisopropyl benzene in 5490 g (45 mols) of 2,4-dimethyl phenol is added dropwise with stirring over a period of 9 to 10 hours at 150° C in a nitrogen atmosphere to a solution of 1830 g (15 mols) of 2,4-dimethyl phenol. At the same time, about 200 to 210 g of water distilled over. The reaction mixture is stirred for 15 minutes, the catalyst is neutralised with 6.5 g of soda and freed from 2,4-dimethyl phenol under reduced pressure up to a sump temperature of 140° C/12 Torr. This leaves a light, crystallising residue of 2230 g (93% of the theoretical). The recrystallisation of 100 g from 150 ml of tetrachloroethane gives α,α'-bis-(2-hydroxy-3,5-dimethyl phenyl-p-diisopropyl benzene in a yield of 80% (melting point 179° C).

후처리

  1. distillationAt the same time, about 200 to 210 g of water distilled over
  2. customfreed from 2,4-dimethyl phenol under reduced pressure up to a sump temperature of 140° C/12 Torr
  3. customThis leaves a light
  4. customcrystallising residue of 2230 g (93% of the theoretical)
  5. customThe recrystallisation of 100 g from 150 ml of tetrachloroethane

출처 및 근거

ORD 기록
ord-992788b060484353b8d14f60c03c76c7
출처 데이터셋
uspto-grants-1978_09
특허 번호
US04116932

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