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Benzaldehyde → HCID 86746675、化合物

HRID 2226990
ノート
印刷プレビュー

反応式

HRID 2226990 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

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

生成物 1

HCID 86746675HCID 86746675、化合物収率 95.9%

反応条件

温度
23 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bdb0c26448fb432ea61749b5e0ef5af5
出典データセット
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05350851

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート