Sodium Hydroxide → Benzofuran, 2,3-dihydro-2,2,4,6,7-pentamethyl-3-(4-methylphenyl)-

HRID 1797402ノート

反応式

HRID 1797402 の反応式
FC(F)(F)S(O)(=O)=O.[CH3:9][C:10]([O:21][C:22]1[CH:27]=[C:26]([CH3:28])[CH:25]=[C:24]([CH3:29])[C:23]=1[CH3:30])([CH3:20])[CH:11]([C:13]1[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=1)O.[OH-].[Na+]>C1(C)C=CC=CC=1>[CH3:9][C:10]1([CH3:20])[CH:11]([C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=2)[C:27]2[C:26]([CH3:28])=[CH:25][C:24]([CH3:29])=[C:23]([CH3:30])[C:22]=2[O:21]1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 62406Trifluoromethanesulfonic acidHCID 9944111HCID 9944111、化合物

生成物 1

HCID 10850374Benzofuran, 2,3-dihydro-2,2,4,6,7-pentamethyl-3-(4-methylphenyl)-収率 74%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
50 °C

実験手順

Trifluoromethanesulfonic acid (7.5 mL) was added to a solution of 2-methyl-1-(4-methylphenyl)-2-(2,3,5-trimethylphenoxy)-1-propanol (253.7 g) obtained in Example 2 in toluene (1260 mL), and the mixture was stirred at 50° C. for 30 minutes and then for 1 hour under reflux. To the mixture was added 1N NaOH (756 mL) at 25° C. The toluene layer was separated and washed with water, and the solvent was distilled off. The residue was dissolved in isopropanol (1511 mL) and water (756 mL) was added thereto. Precipitated crystals were filtered to obtain the title compound (176.33 g, 74%).

後処理

  1. temperaturefor 1 hour under reflux
  2. customThe toluene layer was separated
  3. washwashed with water
  4. distillationthe solvent was distilled off
  5. dissolutionThe residue was dissolved in isopropanol (1511 mL)
  6. additionwater (756 mL) was added
  7. customPrecipitated crystals
  8. filtrationwere filtered

出典と根拠

ORDレコード
ord-57282e67dd504871bf1327fcf527d93b
出典データセット
uspto-grants-2006_04
特許番号
US07034166B2

反応ノート

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