Ethylenediamine → 2-Piperazinone, 3,3-dimethyl-

HRID 43140

反応式

HRID 43140 の反応式
C(O[C:4](=[O:9])[C:5](Br)([CH3:7])[CH3:6])C.[CH2:10]([NH2:13])[CH2:11][NH2:12].C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[CH3:7][C:5]1([CH3:6])[NH:13][CH2:10][CH2:11][NH:12][C:4]1=[O:9]

参加物

5

反応物 3

HCID 3301EthylenediamineHCID 11430Potassium CarbonateHCID 11745Propanoic acid, 2-bromo-2-methyl-, ethyl ester

生成物 1

HCID 2111572-Piperazinone, 3,3-dimethyl-収率 68.8%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
115 °C

実験手順

A solution of ethyl-2-bromoisobutyrate (24 mL, 161 mmol) in toluene (150 mL) was added to a mixture of ethylene diamine (70 mL, 1046 mmol, 6.5 equiv) and potassium carbonate (24.4 g, 177 mmol, 1.1 equiv) in toluene (150 mL). The reaction mixture was heated for 20 h at 115° C., cooled and filtered. The filtrate was concentrated and the residue triturated in Et2O to afford 14.2 g of the title compound as a yellow solid: ESI-MS: 129.1 [M+H]+.

後処理

  1. temperaturecooled
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated
  4. customthe residue triturated in Et2O

出典と根拠

ORDレコード
ord-b6f1359851554a6e8633af1cffc9717a
出典データセット
uspto-grants-2013_09
特許番号
US08536175B2

関連ノート

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