Formic Acid → N-Formyl-L-valine

HRID 595530ノート

反応式

HRID 595530 の反応式
[C:1](OC(=O)C)(=[O:3])C.[NH2:8][C@H:9]([C:13]([OH:15])=[O:14])[CH:10]([CH3:12])[CH3:11].C(O)=O>>[CH:1]([NH:8][C@H:9]([C:13]([OH:15])=[O:14])[CH:10]([CH3:12])[CH3:11])=[O:3]

参加物

4

反応物 3

HCID 284Formic AcidHCID 6287L-ValineHCID 7918Acetic Anhydride

生成物 1

HCID 6950945N-Formyl-L-valine

実験手順

Acetic anhydride (4 mL, 0.04 mol) was added dropwise to a solution of L-Valine (1 g, 8.35 mmol) in formic acid (12 mL, 0.32 mol) while stirring on ice. The mixture was then warmed up to RT and kept stirring for 24 hours before the solvent was removed by rotary evaporation under high vacuum. The formyl-valine was recrystallized from ethyl acetate and the desired product was obtained as a white solid. Yield: 0.78 g (64%) 1HNMR (500 MHz, [D6]Acetone, 25° C., TMS): δ=8.22 (s, 1H), 7.41 (b, 1H), 4.50 (m, 1H), 2.22 (m, 1H), 0.98 (m, 6H).

後処理

  1. stirringkept stirring for 24 hours before the solvent
  2. customwas removed by rotary evaporation under high vacuum
  3. customThe formyl-valine was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-cdbce83ac5c0480294fc2152e54b4207
出典データセット
uspto-grants-2016_01
特許番号
US09243037B2

反応ノート

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