Methanol → HCID 18614386, 화합물

HRID 1725755노트

반응식

HRID 1725755 반응식
[CH2:1]=[C:2]1[CH2:6][CH2:5][C:4]([CH:11]([CH3:13])[CH3:12])([C:7]([O:9]C)=[O:8])[CH2:3]1.O.[OH-].[Li+].CO>O1CCOCC1.O>[CH2:1]=[C:2]1[CH2:6][CH2:5][C:4]([CH:11]([CH3:13])[CH3:12])([C:7]([OH:9])=[O:8])[CH2:3]1

참가 물질

6

반응물 3

HCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 18614378HCID 18614378, 화합물

생성물 1

HCID 18614386HCID 18614386, 화합물수율 111.9%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

반응 조건

온도
80 °C

실험 절차

A solution of the methyl 3-methylene-1-isopropylcyclopentanecarboxylate (Step A, 1.21 g, 6.64 mmol) in a mixture of dioxane (4 mL) and water (4 mL) containing 1.114 g (26.56 mmol) of lithium hydroxide monohydrate was homogenized with methanol, and stirred at 80° C. for 48 hrs. The solvent was removed in vacuo, the residue was dissolved in water and the non-acidic components were extracted with diethyl ether (3×30 mL), combined ethers were back-washed with water (1×30 mL). The combined aqueous phases were acidified with 2N HCl and extracted with chloroform (6×30 mL), dried (anhydrous magnesium sulfate) and evaporated to dryness to leave 1.25 g of crude acid. It was used in the next reaction step without any further purification.

후처리

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in water
  3. extractionthe non-acidic components were extracted with diethyl ether (3×30 mL)
  4. washwere back-washed with water (1×30 mL)
  5. extractionextracted with chloroform (6×30 mL)
  6. dry with materialdried (anhydrous magnesium sulfate)
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-13ad3a811faf4546bc435ea116070bbc
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07491737B2

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