Isobutyraldehyde → HCID 54168338, 화합물

HRID 880420노트

반응식

HRID 880420 반응식
[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]

참가 물질

6

반응물 2

HCID 6561IsobutyraldehydeHCID 7764Ethyl cyanoacetate

생성물 1

HCID 54168338HCID 54168338, 화합물수율 43.9%

시약·촉매·용매 3

HCID 8082Piperidine촉매HCID 176Acetic Acid용매2회HCID 962Water용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-30d04bfd35874d59bec03a29893d4528
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993574B2

반응 노트

불러오는 중…