Hydrochloric Acid → 4-Acetoxy-2-methyl-2-buten-1-ol

HRID 21846

반응식

HRID 21846 반응식
C(=O)(O)[O-].[Na+].C([O:8][CH2:9][C:10]([CH3:17])=[CH:11][CH2:12][O:13][C:14](=[O:16])[CH3:15])=O.O.Cl>CO.C(OCC)(=O)C>[C:14]([O:13][CH2:12][CH:11]=[C:10]([CH3:17])[CH2:9][OH:8])(=[O:16])[CH3:15]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 516892Sodium BicarbonateHCID 543352444-Acetoxy-2-methyl-2-buten-1-ol formate

생성물 1

HCID 5382224-Acetoxy-2-methyl-2-buten-1-ol수율 97.7%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

Sodium bicarbonate (0.40 g, 4.75 mmol, 10 mol %) was added to a solution of 4-acetoxy-2-methyl-2-buten-1-ol formate (8.18 g, 47.5 mmol) in methanol (40 ml). The mixture was stirred at room temperature for 2 hours. After completion of the reaction, most of the methanol was evaporated under reduced pressure. The resulting reaction mixture was poured into a mixture of ice-cooled water (20 ml) and ethyl acetate (100 ml). The pH of the aqueous layer was adjusted to 5 to 6 with 1N hydrochloric acid, and the ethyl acetate layer was separated. The aqueous layer was extracted with ethyl acetate (50 ml) twice. The ethyl acetate layers were combined and dried over anhydrous sodium sulfate. Evaporation of the ethyl acetate gave 4-acetoxy-2-methyl-2-buten-1-ol (6.69 g, 46.4 mmol; Yield: 97.7%) as an oil.

후처리

  1. customAfter completion of the reaction
  2. custommost of the methanol was evaporated under reduced pressure
  3. customThe resulting reaction mixture
  4. additionwas poured into a mixture of ice-
  5. customthe ethyl acetate layer was separated
  6. extractionThe aqueous layer was extracted with ethyl acetate (50 ml) twice
  7. dry with materialdried over anhydrous sodium sulfate
  8. customEvaporation of the ethyl acetate

출처 및 근거

ORD 기록
ord-e443ffc7c83743028b9c10548e7baa67
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424478

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