Nitromethane → HCID 11275397、化合物

HRID 458007ノート

反応式

HRID 458007 の反応式
[NH:1]1[C:5]([CH2:6][C:7]2(C#N)[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)=NN=N1.[N+:15]([CH3:18])([O-:17])=[O:16].[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O1CCCC1.C(OCC)(=O)C>[N+:15]([CH2:18][C:7]1([CH2:6][C:5]#[N:1])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1)([O-:17])=[O:16]

参加物

6

反応物 3

HCID 6375NitromethaneHCID 2724141Tetrabutylammonium FluorideHCID 178509433HCID 178509433、化合物2 回

生成物 1

HCID 11275397HCID 11275397、化合物収率 71%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

The nitrile (compound 2, 0.78 g, 6.44 mmol), nitromethane (0.80 g, 13.11 mmol) and tetrabutyl ammonium fluoride (1.0 M in tetrahydrofuran, 10 mL, 10 mmol) were heated in 20 mL tetrahydrofuran to 70° C. overnight. The reaction mixture was diluted with ethyl acetate and washed with dilute hydrochloric acid and water, dried over magnesium sulphate, filtered, and evaporated to dryness. The residue was purified by chromatography on silica eluting with heptane/ethyl acetate 3:1 to give the required product as a yellow oil (0.83 g, 71%).

後処理

  1. washwashed with dilute hydrochloric acid and water
  2. dry with materialdried over magnesium sulphate
  3. filtrationfiltered
  4. customevaporated to dryness
  5. customThe residue was purified by chromatography on silica eluting with heptane/ethyl acetate 3:1

出典と根拠

ORDレコード
ord-93d5e0f6971d4be6ad999c693711a8f2
出典データセット
uspto-grants-2007_03
特許番号
US07189747B2

反応ノート

読み込み中…