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

HRID 366902

반응식

HRID 366902 반응식
[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)C>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]

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 2631-ButanolHCID 712FormaldehydeHCID 8148DibutylamineHCID 1190244-Hydroxy-2,3,6-trimethylphenyl acetate

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

4-Acetoxy-2,3,5-trimethylphenol (1.8 g; 9.3 mmol), 87.3% paraformaldehyde (0.38 g; 11.2 mmol), 1-butanol (4.48 g; 60.5 mmol), dibutylamine (0.12 g; 0.93 mmol) and acetic acid (0.28 g; 4.7 mmol) were mixed together, then the mixture was reacted under reflux with stirring for 7 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.

후처리

  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

출처 및 근거

ORD 기록
ord-00655e50a3b043d9807a384c2f6ea437
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06130341

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