Hydrochloric Acid → 4-Hydroxy-4-methylcyclohexanone

HRID 509282노트

반응식

HRID 509282 반응식
[CH3:1][C:2]1([OH:12])[CH2:11][CH2:10][C:5]2(OCC[O:6]2)[CH2:4][CH2:3]1.Cl>C1COCC1>[OH:12][C:2]1([CH3:1])[CH2:11][CH2:10][C:5](=[O:6])[CH2:4][CH2:3]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 187130758-Methyl-1,4-dioxaspiro(4.5)decan-8-ol

생성물 1

HCID 285394-Hydroxy-4-methylcyclohexanone수율 92%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

8-Methyl-1,4-dioxaspiro[4.5]decane-8-ol (650 mg, 3.77 mmol) was dissolved in THF (10 ml), followed by addition of 1N aqueous HCl solution (5 ml), and then the resulting mixture was stirred at room temperature for 6 hours. The resulting reaction liquid was concentrated under reduced pressure, and then extracted with 10% MeOH/MC (20 ml×5). The organic layer was dried over anhydrous sodium sulfate, followed by filtration and concentration, and then the residue thus obtained was subjected to MPLC (50% EtOAc/Hexanes), to obtain 443 mg of yellow oil (92%).

후처리

  1. customThe resulting reaction liquid
  2. concentrationwas concentrated under reduced pressure
  3. extractionextracted with 10% MeOH/MC (20 ml×5)
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. filtrationfollowed by filtration and concentration
  6. customthe residue thus obtained

출처 및 근거

ORD 기록
ord-4c8d104f2237465ead45294b8349f757
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096571B2

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