Diethyl (ethoxymethylene)malonate → HCID 178469787、化合物

HRID 574659

反応式

HRID 574659 の反応式
[Na].[CH2:2]([O:9][CH2:10][C:11]([NH2:13])=[NH:12])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C([O:16][CH:17]=[C:18]([C:24](OCC)=O)[C:19]([O:21][CH2:22][CH3:23])=[O:20])C>CCO>[CH2:2]([O:9][CH2:10][C:11]1[N:13]=[C:17]([OH:16])[C:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:24][N:12]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 6871Diethyl (ethoxymethylene)malonateHCID 4164062-PhenylmethoxyethanimidamideHCID 5360545Sodium

生成物 1

HCID 178469787HCID 178469787、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Sodium (4.6 g, 200 mmol) was added to EtOH (500 mL) and the mixture was stirred until a clear solution was obtained. Then, step B product, 2-c, (20.1 g, 100 mmol) and diethyl 2-(ethoxymethylene)malonate (21.6 g, 100 mmol) were added to the clear mixture, respectively. The reaction mixture was refluxed overnight and then concentrated under vacuum, washed with EA. The wet cake was then dried to afford compound 2-d (40.0 g, crude). LC-MS: (M+H)+ 289. The crude was directly used to next step without further purification.

後処理

  1. customwas obtained
  2. temperatureThe reaction mixture was refluxed overnight
  3. concentrationconcentrated under vacuum
  4. washwashed with EA
  5. customThe wet cake was then dried
  6. customto afford compound 2-d (40.0 g, crude)
  7. customThe crude was directly used to next step without further purification

出典と根拠

ORDレコード
ord-941e7dbe208c45f5adc496c3dd093870
出典データセット
uspto-grants-2015_05
特許番号
US09034851B2

関連ノート

読み込み中…