Ethyl 2-(benzylamino)propanoate → Methyl 4-(benzyl(1-ethoxy-1-oxopropan-2-yl)amino)butanoate

HRID 450227

反応式

HRID 450227 の反応式
[CH2:1]([O:3][C:4](=[O:15])[CH:5]([NH:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH3:6])[CH3:2].O=[C:17]([CH2:22][CH3:23])[C:18]([O:20][CH3:21])=[O:19]>ClCCCl>[CH3:21][O:20][C:18](=[O:19])[CH2:17][CH2:22][CH2:23][N:7]([CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[CH:5]([C:4]([O:3][CH2:1][CH3:2])=[O:15])[CH3:6]

参加物

4

反応物 2

HCID 222273Ethyl 2-(benzylamino)propanoateHCID 5451272-Ketobutyric acid methyl ester

生成物 1

HCID 67423852Methyl 4-(benzyl(1-ethoxy-1-oxopropan-2-yl)amino)butanoate

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

2-Benzylamino-propionic acid ethyl ester (1.4 g, 6.7 mmol), methyl oxo-butanoate (1.7 g, 13.5 mmol), LEA (1.9 mL, 13.5 mmol) and NaBH(Oac)3 (2.9 g, 13.5 mmol) are taken up in 1,2-DCE (35 mL) and stirred at rt for 4 h. The reaction is partitioned between DCM and saturated aqueous NaHCO3. The organic layer is removed, dried over anhydrous Na2SO4, and concentrated in vacuo. The crude residue is used without further purification. MS (ESI) m/z 308.3 (M+1).

後処理

  1. customThe reaction is partitioned between DCM and saturated aqueous NaHCO3
  2. customThe organic layer is removed
  3. dry with materialdried over anhydrous Na2SO4
  4. concentrationconcentrated in vacuo
  5. customThe crude residue is used without further purification

出典と根拠

ORDレコード
ord-706097fb77c34eac9dcbb05dff386e10
出典データセット
uspto-grants-2013_07
特許番号
US08486954B2

関連ノート

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