N-Methylaniline → (Methyl-phenyl-amino)-acetic acid ethyl ester

HRID 1005269

反応式

HRID 1005269 の反応式
Br[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].[CH3:8][NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(N(CC)C(C)C)(C)C>C(#N)C.CCOCC>[CH3:8][N:9]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4]

参加物

6

反応物 3

HCID 7515N-MethylanilineHCID 7748Ethyl bromoacetateHCID 81531Diisopropylethylamine

生成物 1

HCID 265936(Methyl-phenyl-amino)-acetic acid ethyl ester

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6342Acetonitrile溶媒

実験手順

A solution of 16.7 g (100 mmol) of ethyl bromoacetate, 10.7 g (100 mmol) of N-methylaniline, and 12.9 g (100 mmol) of N,N-diisopropylethylamine in 100 mL of acetonitrile was allowed to stand for 24 hr. and then diluted with 200 ml of ether. The amine salt was filtered and the filtrate concentrated, dissolved in 150 ml of CH2Cl2, washed with water, filtered through a plug of sodium sulfate/silica and distilled: 15.5 g (80%), b.p. 132°/12 mm.

後処理

  1. filtrationThe amine salt was filtered
  2. concentrationthe filtrate concentrated
  3. dissolutiondissolved in 150 ml of CH2Cl2
  4. washwashed with water
  5. filtrationfiltered through a plug of sodium sulfate/silica
  6. distillationdistilled

出典と根拠

ORDレコード
ord-43b4e9700bb941738da9a22017179fa1
出典データセット
uspto-grants-2000_04
特許番号
US06054260

関連ノート

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