Water → 7-(2-Hydroxy-3,4,6-trimethylphenyl)-7-phenylheptanoic acid

HRID 2254350노트

반응식

HRID 2254350 반응식
[C:1]1([CH:7]=[CH:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([OH:15])=[O:14])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:16][C:17]1[C:22]([CH3:23])=[CH:21][C:20]([CH3:24])=[CH:19][C:18]=1O.CS(O)(=O)=O.[OH2:31]>ClCCl>[OH:31][C:18]1[C:17]([CH3:16])=[C:22]([CH3:23])[CH:21]=[C:20]([CH3:24])[C:19]=1[CH:7]([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([OH:15])=[O:14]

참가 물질

6

반응물 4

HCID 962WaterHCID 6395Methanesulfonic AcidHCID 127692,3,5-TrimethylphenolHCID 539006207-Phenyl-6-heptenoic acid

생성물 1

HCID 145139667-(2-Hydroxy-3,4,6-trimethylphenyl)-7-phenylheptanoic acid수율 85.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
25 °C

실험 절차

7-Phenyl-6-heptenoic acid (10 g) and 2,3,5-trimethylphenol (8.3 g) were suspended in dichloromethane (80 ml). To the suspension was added dropwise methanesulfonic acid (9.4 g) at a temperature ranging from 17°-25° C. The mixture was stirred at 25° C. for 6 hours, to which was then added water (80 ml). The dichloromethane layer was separated and washed with water three times. Dichloromethane was distilled off under reduced pressure, and the residue was recrystallized from toluene (38 m;) to give 7-(2-hydroxy-3,4,6-trimethylphenyl)-7-phenylheptanoic acid (14.2g, 85.2%) as white crystals.

후처리

  1. customranging from 17°-25° C
  2. customThe dichloromethane layer was separated
  3. washwashed with water three times
  4. distillationDichloromethane was distilled off under reduced pressure
  5. customthe residue was recrystallized from toluene (38 m;)

출처 및 근거

ORD 기록
ord-e69a5bd50ae546f3ad9e8375f5f95afc
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05235091

반응 노트

불러오는 중…