Phenol → Benzoic acid, 3,5-dimethyl-, methyl ester

HRID 861679

반응식

HRID 861679 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([CH3:12])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].[C:13]1(O)[CH:18]=[CH:17]C=[CH:15][CH:14]=1>[O-]C1C=CC=CC=1.[O-]C1C=CC=CC=1.[O-]C1C=CC=CC=1.[O-]C1C=CC=CC=1.[Ti+4].C1(O)C=CC=CC=1>[CH3:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([CH3:12])[CH:11]=1)[C:5]([O:7][C:8]1[CH:17]=[CH:18][CH:13]=[CH:14][CH:15]=1)=[O:6].[CH3:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([CH3:12])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6]

참가 물질

5

반응물 2

HCID 996Phenol2회HCID 32786Benzoic acid, 3,5-dimethyl-, methyl ester

생성물 2

HCID 32786Benzoic acid, 3,5-dimethyl-, methyl esterHCID 19704462Phenyl 3,5-dimethylbenzoate

시약·촉매·용매 1

HCID 86752029Titanium tetraphenoxide phenol촉매

실험 절차

Into this autoclave were charged methyl 3,5-dimethylbenzoate 90 g (550 mmole), phenol 207 g (2200 mmole) and titanium tetraphenoxide/phenol adduct 2.8 g (5.5 mmole) in a state such that the phenol was melting. The autoclave was sealed and then cooled with ice. After sufficient cooling, the inner gas was evacuated with a vacuum pump. Then, the contents were heated and reacted for three hours at 230° C. Furthermore, during the reaction, the liquid held in the reservoir was continuously removed with a pump at a rate of 10 g per hour. After cooling, the reaction mixture in the autoclave was separated by distillation to obtain phenyl 3,5-dimethylbenzoate (product) in an amount of 85 g (68% yield in terms of methyl 3,5-dimethylbenzoate). The boiling point was 155° C./2 mmHg, and the melting point was 32° C.

후처리

  1. customThe autoclave was sealed
  2. temperaturecooled with ice
  3. customAfter sufficient cooling, the inner gas was evacuated with a vacuum pump
  4. temperatureThen, the contents were heated
  5. customreacted for three hours at 230° C
  6. customFurthermore, during the reaction
  7. customwas continuously removed with a pump at a rate of 10 g per hour
  8. temperatureAfter cooling
  9. customthe reaction mixture in the autoclave was separated by distillation

출처 및 근거

ORD 기록
ord-e6cbd8c2ee7a4e58a36f8c4288f0b247
출처 데이터셋
uspto-grants-1998_02
특허 번호
US05714627

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