Lithium Hydroxide → HCID 18628853, 화합물

HRID 1060732노트

반응식

HRID 1060732 반응식
[CH:1]1([CH2:7][CH:8]([C:14]([O:16]CC)=[O:15])[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[OH-].[Li+]>C(O)C.O>[CH:1]1([CH2:7][CH:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[C:14]([OH:16])=[O:15])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 599487Diethyl 2-cyclohexylmethylmalonate

생성물 1

HCID 18628853HCID 18628853, 화합물수율 74%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A solution comprised of diethyl 2-cyclohexylmethylmalonate (12.817 g, 50 mmol) in ethanol (100 mL) was treated with a solution of comprised of lithium hydroxide (1.198 g, 50 mmol) in water (50 mL) and the mixture was stirred for approximately 12 hours at ambient temperature. Solvent was removed by evaporation and the residue was diluted with water (50 mL). The dilution was extracted with diethyl ether (2×). The aqueous layer was cooled to 0° C., acidified to pH 1.5 with 1N hydrochloric acid (50 mL), saturated with solid sodium chloride and then extracted with ethyl acetate (2×). The combined ethyl acetate extracts were dried (MgSO4) and concentrated. The residue was dried to provide 3-cyclohexyl-2-ethoxycarbonylpropionic acid (8.52 g, 37 mmol) as an oil.

후처리

  1. additionwas treated with a solution
  2. customSolvent was removed by evaporation
  3. additionthe residue was diluted with water (50 mL)
  4. extractionThe dilution was extracted with diethyl ether (2×)
  5. temperatureThe aqueous layer was cooled to 0° C.
  6. extractionextracted with ethyl acetate (2×)
  7. dry with materialThe combined ethyl acetate extracts were dried (MgSO4)
  8. concentrationconcentrated
  9. customThe residue was dried

출처 및 근거

ORD 기록
ord-becbf32b2d8c4bc9abc5bc8a5b2471ba
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525036B2

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