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Benzaldehyde → HCID 86746675, 화합물

HRID 2226990
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HRID 2226990 반응식
[CH:1](=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:10][C@H:11]([C:15]([NH2:17])=[O:16])[CH2:12][CH2:13][CH3:14].CCN(CC)CC>>[CH:1](=[N:17][C:15](=[O:16])[C@H:11]([CH2:12][CH2:13][CH3:14])[NH2:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 240BenzaldehydeHCID 8471TriethylamineHCID 56777018(2S)-2-aminopentanamide hydrochloride

생성물 1

HCID 86746675HCID 86746675, 화합물수율 95.9%

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온도
23 °C

실험 절차

Fresh benzaldehyde (4.02 g, 37.9 mmol) was added to a slurry of 4.0 g L-norvalinamide-HCl (XII) (26.2 mmol) in 70 mL 1-PrOH, followed by 4.08 mL Et3N (29.3 mmol). The mixture, which became clear after stirring at 23° C. for 70 minutes, was then evaporated to 15 mL, and 175 mL Et2O added. After filtration, the precipitated salts were washed with additional Et2O, solvent evaporated from the combined filtrate, and residual benzaldehyde removed under high vacuum to give 5.13 g N-benzylidene-L-norvalinamide (XIII) as a light yellow solid (UV λmax =249 nm in MeOH). The purity of this material was determined by normal phase HPLC.

후처리

  1. customwas then evaporated to 15 mL, and 175 mL Et2O
  2. additionadded
  3. filtrationAfter filtration
  4. washthe precipitated salts were washed with additional Et2O, solvent
  5. customevaporated from the combined filtrate, and residual benzaldehyde
  6. customremoved under high vacuum

출처 및 근거

ORD 기록
ord-bdb0c26448fb432ea61749b5e0ef5af5
출처 데이터셋
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05350851

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