Sulfuric Acid → 1,4-Diacetoxy-2,6-di-tert-butylbenzene

HRID 23805

反応式

HRID 23805 の反応式
[C:1]([C:5]1[CH:11]=[C:10]([OH:12])[CH:9]=[C:8]([C:13]([CH3:16])([CH3:15])[CH3:14])[C:6]=1[OH:7])([CH3:4])([CH3:3])[CH3:2].CCCC[CH2:21][CH3:22].[C:23](OC(=O)C)(=[O:25])[CH3:24].S(=O)(=O)(O)[OH:31]>C(OCC)(=O)C.O>[C:23]([O:7][C:6]1[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])=[CH:11][C:10]([O:12][C:21](=[O:31])[CH3:22])=[CH:9][C:8]=1[C:13]([CH3:16])([CH3:15])[CH3:14])(=[O:25])[CH3:24]

参加物

7

反応物 4

HCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 8058HexaneHCID 755502,6-Di-tert-butylhydroquinone

生成物 1

HCID 126344621,4-Diacetoxy-2,6-di-tert-butylbenzene

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

To the 2,6-di-tert-butylhydroquinone obtained in Example 10, 50 mL of hexane, 13.92 g (136.5 mmol) of acetic anhydride and 0.79 g (8.06 mmol) of sulfuric acid were added and the mixture was stirred for 2 hours at 50° C. The mixture was cooled to 10° C. and after adding 30 mL of water and 10 mL of ethyl acetate, the mixture was stirred overnight. The solution was subjected to liquid-liquid separation and the aqueous layer was discarded; thereafter, the organic layer was washed with 40 mL of 7.5% aqueous sodium hydrogencarbonate and 40 mL of 10% aqueous sodium chloride and the solvent was distilled off under reduced pressure to give 1,4-diacetoxy-2,6-di-tert-butylbenzene.

後処理

  1. temperatureThe mixture was cooled to 10° C.
  2. stirringthe mixture was stirred overnight
  3. customThe solution was subjected to liquid-liquid separation
  4. washthereafter, the organic layer was washed with 40 mL of 7.5% aqueous sodium hydrogencarbonate and 40 mL of 10% aqueous sodium chloride
  5. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-6e941d7d62d446969ab06bbadee4016b
出典データセット
uspto-grants-2005_02
特許番号
US06852867B2

関連ノート

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