Methyl 2-(methyl(4-nitrobenzyl)amino)acetate → HCID 18472314、化合物

HRID 1277237ノート

反応式

HRID 1277237 の反応式
[CH3:1][O:2][C:3](=[O:17])[CH2:4][N:5]([CH2:7][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][CH:9]=1)[CH3:6]>C(O)(=O)C>[CH3:1][O:2][C:3](=[O:17])[CH2:4][N:5]([CH2:7][C:8]1[CH:9]=[CH:10][C:11]([NH2:14])=[CH:12][CH:13]=1)[CH3:6]

参加物

3

反応物 1

HCID 18472662Methyl 2-(methyl(4-nitrobenzyl)amino)acetate

生成物 1

HCID 18472314HCID 18472314、化合物収率 57.6%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

In acetic acid (100 ml) was dissolved N-(4-nitrobenzyl)sarcosine methyl ester (5.96 g), and to the mixture was added little by little reduced iron (7 g). The mixture was stirred at room temperature overnight. The solvent was evaporated, and to the residue was added ethyl acetate. The precipitates were filtered off, and the filtrate was washed with sodium hydroxide solution, water and saturated brine, and dried with anhydrous magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the resulting residue was purified with silica gel column chromatography (ethyl acetate/hexane) to give N-(4-aminobenzyl)sarcosine methyl ester (3.0 g) as red oil.

後処理

  1. customThe solvent was evaporated
  2. additionto the residue was added ethyl acetate
  3. filtrationThe precipitates were filtered off
  4. washthe filtrate was washed with sodium hydroxide solution, water and saturated brine
  5. dry with materialdried with anhydrous magnesium sulfate
  6. customUnder reduced pressure, the solvent was evaporated
  7. customthe resulting residue was purified with silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-e018448e98c845009b33a4748ef175af
出典データセット
uspto-grants-2000_12
特許番号
US06166006

反応ノート

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