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

HRID 2254350ノート

反応式

HRID 2254350 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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;)

出典と根拠

ORDレコード
ord-e69a5bd50ae546f3ad9e8375f5f95afc
出典データセット
uspto-grants-1993_08
特許番号
US05235091

反応ノート

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