Methyl bromoacetate → HCID 14402229、化合物

HRID 1382183ノート

反応式

HRID 1382183 の反応式
Br[CH2:2][C:3]([O:5][CH3:6])=[O:4].[CH2:7]([NH:9][C:10]1[CH:11]=[C:12]([OH:16])[CH:13]=[CH:14][CH:15]=1)[CH3:8].C(N(C(C)C)C(C)C)C>C1(C)C=CC=CC=1>[CH3:6][O:5][C:3](=[O:4])[CH2:2][N:9]([CH2:7][CH3:8])[C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([OH:16])[CH:11]=1

参加物

5

反応物 3

HCID 60984Methyl bromoacetateHCID 81531DiisopropylethylamineHCID 5789913-Ethylaminophenol

生成物 1

HCID 14402229HCID 14402229、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

Methyl bromoacetate (10.7 g, 70 mmole), 3-(ethylamino) phenol from above (4.8 g, 35 mmole), and ethyl diisopropyl amine (4.45 g, 35 mmole) were combined in 25 ml of toluene. The mixture was heated at 100° C. for 30 min. and then evaporated under vacuum and chromatographed on a silica gel column using 5% (v/v) methanol/methylene chloride. The combined fractions were washed with saturated sodium bicarbonate and neutralized with 0.1N HCL. The combined fractions were dried over Na2SO4 and evaporated to give 7.24 g of N-ethyl-N-3-hydroxyphenyl glycine methyl ester.

後処理

  1. customevaporated under vacuum
  2. customchromatographed on a silica gel column
  3. washThe combined fractions were washed with saturated sodium bicarbonate and neutralized with 0.1N HCL
  4. dry with materialThe combined fractions were dried over Na2SO4
  5. customevaporated

出典と根拠

ORDレコード
ord-ccf382539ac54e4c9c90bea6fd1e7c0a
出典データセット
uspto-grants-1989_02
特許番号
US04806488

反応ノート

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