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

HRID 1005269

반응식

HRID 1005269 반응식
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]

참가 물질

6

반응물 3

HCID 7515N-MethylanilineHCID 7748Ethyl bromoacetateHCID 81531Diisopropylethylamine

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-43b4e9700bb941738da9a22017179fa1
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06054260

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