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Triethylamine → N-butyloxycarbonyl-amino malonic acid diethyl ester

HRID 487335
ノート
印刷プレビュー

反応式

HRID 487335 の反応式
Cl.[CH2:2]([O:4][C:5](=[O:11])[CH:6]([NH2:10])[C:7]([OH:9])=[O:8])[CH3:3].[CH2:12]([O:16][C:17](Cl)=[O:18])[CH2:13][CH2:14][CH3:15].[CH2:20](N(CC)CC)[CH3:21]>C(Cl)Cl>[CH2:2]([O:4][C:5](=[O:11])[CH:6]([NH:10][C:17]([O:16][CH2:12][CH2:13][CH2:14][CH3:15])=[O:18])[C:7]([O:9][CH2:20][CH3:21])=[O:8])[CH3:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 61140Butyl chloroformateHCID 20464734Ethyl aminomalonate hydrochloride

生成物 1

HCID 21805915N-butyloxycarbonyl-amino malonic acid diethyl ester収率 96.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
20 °C

実験手順

To an ice-cold suspension of 15 g (70.87 mmol) of amino malonic acid ethyl ester hydrochloride in 180 ml of methylene chloride, 10.8 g (75 mmol) of chloroformic acid butyl ester and then 14.7 g (145 mmol) of triethylamine were added within several minutes. In this case the temperature was constantly maintained under 20° C. After the addition was completed, the reaction was stirred for another 75 minutes at room temperature. The reaction solution was diluted with 80 ml of CH2Cl2, washed with two portions of water, and dried on Na2SO4. After concentration by evaporation on a rotary evaporator, 18.8 g (96 percent) of pure title product was obtained. Other data concerning the product was:

後処理

  1. additionAfter the addition
  2. washwashed with two portions of water
  3. customdried on Na2SO4
  4. concentrationAfter concentration
  5. customby evaporation
  6. customon a rotary evaporator

出典と根拠

ORDレコード
ord-b322bd32afe2486a89381f5cb94636c0
出典データセット
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05294710

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート