Isobutyraldehyde → HCID 54168338、化合物

HRID 880420ノート

反応式

HRID 880420 の反応式
[CH3:1][CH2:2][O:3][C:4]([CH2:6][C:7]#[N:8])=[O:5].[CH:9](=O)[CH:10]([CH3:12])[CH3:11]>C(O)(=O)C.O.N1CCCCC1>[C:7]([C:6](=[CH:9][CH:10]([CH3:12])[CH3:11])[C:4]([O:3][CH2:2][CH3:1])=[O:5])#[N:8]

参加物

6

反応物 2

HCID 6561IsobutyraldehydeHCID 7764Ethyl cyanoacetate

生成物 1

HCID 54168338HCID 54168338、化合物収率 43.9%

試薬・触媒・溶媒 3

HCID 8082Piperidine触媒HCID 176Acetic Acid溶媒2 回HCID 962Water溶媒

実験手順

A solution of piperidine (0.3 mL, 3.04 mmol) in acetic acid (3 mL) was added to a solution of ethyl cyano acetate (10 g, 88.50 mmol) and isobutyraldehyde (9.35 g, 0.13 mol) in acetic acid at room temperature. The reaction mixture was allowed to stand for 24 h at room temperature, then diluted with water (50 mL) and extracted with ether (3×50 mL). The combined ether layers were washed with saturated bicarbonate solution, water, and brine and the organics were dried over anhydrous sodium sulfate and concentrated under reduced pressure to give the crude compound. Purification by vacuum distillation (95° C. at 0.1 mm Hg) afforded ethyl 2-cyano-4-methyl-pent-2-enoate (6.5 g, 30%) as a liquid.

後処理

  1. extractionextracted with ether (3×50 mL)
  2. washThe combined ether layers were washed with saturated bicarbonate solution, water, and brine
  3. dry with materialthe organics were dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto give the crude compound
  6. customPurification
  7. distillationby vacuum distillation (95° C. at 0.1 mm Hg)

出典と根拠

ORDレコード
ord-30d04bfd35874d59bec03a29893d4528
出典データセット
uspto-grants-2015_03
特許番号
US08993574B2

反応ノート

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