Benzoic Acid → 4-Acetoxy-2,3,5-trimethyl-6-butoxymethyl-1-hydroxybenzene

HRID 368807

反応式

HRID 368807 の反応式
[C:1]([O:4][C:5]1[C:10]([CH3:11])=[CH:9][C:8]([OH:12])=[C:7]([CH3:13])[C:6]=1[CH3:14])(=[O:3])[CH3:2].C=O.[CH2:17]([OH:21])[CH2:18][CH2:19][CH3:20].[CH2:22](NCCCC)CCC.C(O)(=O)C1C=CC=CC=1>C1(C)C=CC=CC=1>[C:1]([O:4][C:5]1[C:10]([CH3:11])=[C:9]([CH2:22][O:21][CH2:17][CH2:18][CH2:19][CH3:20])[C:8]([OH:12])=[C:7]([CH3:13])[C:6]=1[CH3:14])(=[O:3])[CH3:2]

参加物

7

反応物 5

HCID 243Benzoic AcidHCID 2631-ButanolHCID 712FormaldehydeHCID 8148DibutylamineHCID 1190244-Hydroxy-2,3,6-trimethylphenyl acetate

生成物 1

HCID 110332624-Acetoxy-2,3,5-trimethyl-6-butoxymethyl-1-hydroxybenzene

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

4-Acetoxy-2,3,5-trimethylphenol (5.83 g; 30.0 mmol), 87.3% paraformaldehyde (1.24 g; 36.0 mmol), 1-butanol (14.46 g; 195.0 mmol), dibutylamine (0.39 g; 3.0 mmol) and benzoic acid (1.83 g; 15.0 mmol) were mixed together, then the mixture was reacted under reflux with stirring for 6 hours. After completion of the reaction, toluene was added into the resulting mixture for extraction of the resulting product in toluene, and then the toluene phase was separated. After the separated toluene phase was sequentially washed with water, an aqueous 1% dilute sulfuric acid solution, an aqueous 5% sodium hydrogen carbonate solution and water, the toluene phase was distilled under reduced pressure to distill off compounds with low boiling points, to give 4-acetoxy-2,3,5-trimethyl-6-butoxymethyl-1-hydroxybenzene.

後処理

  1. customthe mixture was reacted
  2. temperatureunder reflux
  3. customthe toluene phase was separated
  4. washAfter the separated toluene phase was sequentially washed with water
  5. distillationan aqueous 1% dilute sulfuric acid solution, an aqueous 5% sodium hydrogen carbonate solution and water, the toluene phase was distilled under reduced pressure
  6. distillationto distill off compounds with low boiling points

出典と根拠

ORDレコード
ord-be608c254ed94102b182b843625e0ab7
出典データセット
uspto-grants-2000_10
特許番号
US06133471

関連ノート

読み込み中…