Acetic Acid → HCID 10012389、化合物

HRID 455681ノート

反応式

HRID 455681 の反応式
[OH-].[Na+].[N+:3]([CH3:6])([O-:5])=[O:4].[CH:7]1([CH:13]=[O:14])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1.C(O)(=O)C>CCO>[CH:7]1([CH:13]([OH:14])[CH2:6][N+:3]([O-:5])=[O:4])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 6375NitromethaneHCID 14798Sodium HydroxideHCID 16275Cyclohexanecarboxaldehyde

生成物 1

HCID 10012389HCID 10012389、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

10 M aqueous NaOH (8.31 mL, 83 mmol) was added dropwise via addition funnel to a solution of nitromethane (4.46 mL, 83 mmol) and cyclohexanecarboxaldehyde (10 mL, 83 mmol) in EtOH (20 mL) at 0° C. with vigorous stirring. The resulting white slurry was stirred 10 minutes and became a white solid. Acetic acid (4.76 mL, 83 mmol) was added and the reaction was partitioned between diethyl ether and water. The layers were separated and the aqueous layer was extracted with diethyl ether. The combined organic extracts were washed with water, saturated aqueous sodium chloride, and dried over magnesium sulfate. The solution was filtered and concentrated in vacuo and dried under vacuum to afford 1-cyclohexyl-2-nitroethanol. The product was used directly for the next step without further purification.

後処理

  1. customthe reaction was partitioned between diethyl ether and water
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted with diethyl ether
  4. washThe combined organic extracts were washed with water, saturated aqueous sodium chloride
  5. dry with materialdried over magnesium sulfate
  6. filtrationThe solution was filtered
  7. concentrationconcentrated in vacuo
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-df0f77627fbe4c14a54ce02cef287b20
出典データセット
uspto-grants-2013_07
特許番号
US08497264B2

反応ノート

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