Nitromethane → HCID 11275397、化合物

HRID 722833ノート

反応式

HRID 722833 の反応式
[C:1]1(=[CH:7][C:8]#[N:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[N+:10]([CH3:13])([O-:12])=[O:11].[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O1CCCC1.C(OCC)(=O)C>[N+:10]([CH2:13][C:1]1([CH2:7][C:8]#[N:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)([O-:12])=[O:11]

参加物

6

反応物 3

HCID 6375NitromethaneHCID 97105Acetonitrile, 2-cyclohexylidene-2 回HCID 2724141Tetrabutylammonium Fluoride

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-3c2c532dbaaf4bc1aec9c132c7268d7f
出典データセット
uspto-grants-2006_11
特許番号
US07138542B2

反応ノート

読み込み中…