ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → HCID 19104666、化合物

HRID 1197744
ノート
印刷プレビュー

反応式

HRID 1197744 の反応式
[CH:1]([C:4]1([CH3:17])[NH:8][C:7]([C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][N:10]=2)=[N:6][C:5]1=[O:16])([CH3:3])[CH3:2].C([Li])CCC.C[O:24][C:25](=O)[C:26]([N:28]([CH3:30])[CH3:29])=[O:27].O>O1CCCC1>[CH3:29][N:28]([C:26](=[O:27])[C:25]([C:14]1[C:9]([C:7]2[NH:6][C:5](=[O:16])[C:4]([CH:1]([CH3:3])[CH3:2])([CH3:17])[N:8]=2)=[N:10][CH:11]=[C:12]([CH3:15])[CH:13]=1)=[O:24])[CH3:30]
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

6

反応物 4

HCID 962WaterHCID 13280608Methyl (dimethylamino)(oxo)acetateHCID 178418339ButyllithiumHCID 178423999HCID 178423999、化合物

生成物 1

HCID 19104666HCID 19104666、化合物収率 46%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-70 °C

実験手順

To a stirred solution of 2.5 g (0.011 mole) of 2-(5-isopropyl-5-methyl-4-oxo-2-imidazolin-2 -yl)-5-methyl pyridine in 100 ml of dry tetrahydrofuran cooled to -70° C. under the presence of nitrogen was added dropwise a 9.68 ml of 2.5 molar n-butyllithium, thereby temperature was maintained below -65° C. The solution was stirred at -70° C. for 3 hours and a solution 1.96 g of N,N-dimethyl oxamic acid methyl ester(0.015 mole) in 10 ml of anhydrous tetrahydrofuran was added dropwise while maintaining the temperature below -65° C. After stirring another hour at -70° C., the solution was poured into water and extracted with methylene chloride. The combined organic phases were dried over magnesium sulfate, and evaporated under reduced pressure. Trituration of the residue with diethyl ether affored a crude solid which was recrystallized from a mixture of diethyl ether and methylene chloride to yield 1.67 g of a white solid (m.p=180°-182° C.).

後処理

  1. temperaturetemperature was maintained below -65° C
  2. temperaturewhile maintaining the temperature below -65° C
  3. stirringAfter stirring another hour at -70° C.
  4. extractionextracted with methylene chloride
  5. dry with materialThe combined organic phases were dried over magnesium sulfate
  6. customevaporated under reduced pressure
  7. customwas recrystallized from a mixture of diethyl ether and methylene chloride

出典と根拠

ORDレコード
ord-90376fa523c24266a538b2be35954a68
出典データセット
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05278134

反応ノート

読み込み中…

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