Nitrogen → 4-[(2,4-Dinitro-phenyl)-methyl-carbamoyl]-butyric acid methyl ester

HRID 1967480ノート

反応式

HRID 1967480 の反応式
N#N.[CH3:3][O:4][C:5](=[O:24])[CH2:6][CH2:7][CH2:8][C:9](=[O:23])[NH:10][C:11]1[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][C:12]=1[N+:20]([O-:22])=[O:21].S(OC)(O[CH3:29])(=O)=O.C([O-])([O-])=O.[K+].[K+]>C(#N)C>[CH3:3][O:4][C:5](=[O:24])[CH2:6][CH2:7][CH2:8][C:9](=[O:23])[N:10]([C:11]1[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][C:12]=1[N+:20]([O-:22])=[O:21])[CH3:29]

参加物

6

反応物 4

HCID 947NitrogenHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 866564154-(2,4-Dinitro-phenylcarbamoyl)-butyric acid methyl ester

生成物 1

HCID 583828074-[(2,4-Dinitro-phenyl)-methyl-carbamoyl]-butyric acid methyl ester

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a 100 mL round bottom 3-neck flask equipped with stir bar, thermocouple, and N2 sweep were charged 16.67 g (53.6 mmol) of 4-(2,4-dinitro-phenylcarbamoyl)-butyric acid methyl ester and 50 mL (5 volumes vs. dinitroaniline) of acetonitrile at room temperature. To this clear yellow stirred solution was then added 6.09 mL (8.10 g, 64.2 mmol, 1.2 equiv) of dimethyl sulfate and 14.80 g (107 mmol, 2.0 equiv) of K2CO3. The mixture turned dark reddish orange with the addition and exhibited an exotherm of less than 5° C. The reaction was monitored periodically by HPLC Method A and was complete after 22.5 hours at room temperature.

後処理

  1. customTo a 100 mL round bottom 3-neck flask equipped
  2. additionThe mixture turned dark reddish orange with the addition
  3. customan exotherm of less than 5° C

出典と根拠

ORDレコード
ord-5c7b67086f164b4292894d365813154f
出典データセット
uspto-grants-2013_04
特許番号
US08420829B2

反応ノート

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