Lithium Hydroxide → HCID 18628853、化合物

HRID 1060732ノート

反応式

HRID 1060732 の反応式
[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

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 599487Diethyl 2-cyclohexylmethylmalonate

生成物 1

HCID 18628853HCID 18628853、化合物収率 74%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-becbf32b2d8c4bc9abc5bc8a5b2471ba
出典データセット
uspto-grants-2003_02
特許番号
US06525036B2

反応ノート

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