Water → AC1Lgxvo

HRID 2401263ノート

反応式

HRID 2401263 の反応式
Cl.[NH2:2][C@H:3]([C:7]([NH2:9])=[O:8])[CH:4]([CH3:6])[CH3:5].[C:10](=O)([O-])[OH:11].[Na+].ClC(OC1C=CC([N+]([O-])=O)=CC=1)=O.O>C(#N)C>[CH3:5][CH:4]([C@@H:3]1[NH:2][C:10](=[O:11])[NH:9][C:7]1=[O:8])[CH3:6]

参加物

6

反応物 4

HCID 962WaterHCID 821294-Nitrophenyl chloroformateHCID 516892Sodium BicarbonateHCID 13689583L-Valinamide--hydrogen chloride (1/1)

生成物 1

HCID 853633AC1Lgxvo収率 58%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of L-valinamide hydrochloride (1.0 g) and sodium hydrogen carbonate (3.03 g) in acetonitrile (100 mL) was added p-nitrophenyl chloroformate (1.32 g), and the mixture was stirred at room temperature for 3 hr. Water was added thereto, the resulting mixture was stirred at room temperature overnight, and then acetonitrile was distilled off under reduced pressure. After extraction with ethyl acetate, the organic layer was concentrated under reduced pressure. The residue was purified by column chromatography (silica gel cartridge, chloroform/methanol) to afford (5S)-5-(propan-2-yl)imidazolidine-2,4-dione (540 mg).

後処理

  1. stirringthe resulting mixture was stirred at room temperature overnight
  2. distillationacetonitrile was distilled off under reduced pressure
  3. extractionAfter extraction with ethyl acetate
  4. concentrationthe organic layer was concentrated under reduced pressure
  5. customThe residue was purified by column chromatography (silica gel cartridge, chloroform/methanol)

出典と根拠

ORDレコード
ord-132f745f687b4f7aba5188080f1dee15
出典データセット
uspto-grants-2014_08
特許番号
US08796272B2

反応ノート

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