Hydrochloric Acid → 1-(Pyridin-2-yl)propan-2-one

HRID 900433

反応式

HRID 900433 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH3:7].C([Li])CCC.[CH3:13][C:14](N(C)C)=[O:15].Cl>O1CCCC1.CCCCCC.C(OCC)(=O)C.O>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][C:14](=[O:15])[CH3:13]

参加物

9

反応物 4

HCID 313Hydrochloric AcidHCID 79752-MethylpyridineHCID 31374DimethylacetamideHCID 178418339Butyllithium

生成物 1

HCID 959101-(Pyridin-2-yl)propan-2-one

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒HCID 8058Hexane溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
-75 °C

実験手順

2-Picoline (2 g) was dissolved in tetrahydrofuran (30 ml) and the solution was cooled to −75° C. Butyl lithium (14.73 ml. of a 1.6M-solution in hexane) was added dropwise and the mixture stirred for 2 h. Dimethylacetamide (1.87 ml) was then added dropwise and the reaction was allowed to warm up to room temperature and stirring was continued for a further 2 h. Water (8.6 ml) and 36% hydrochloric acid (1.3 ml) were added and after stirring for another 30 minutes, ethyl acetate was added. The separated solvent phase was washed with brine and then dried (MgSO4). On evaporation an oil was obtained and used without further purification.

後処理

  1. temperatureto warm up to room temperature
  2. stirringstirring
  3. waitwas continued for a further 2 h
  4. stirringafter stirring for another 30 minutes
  5. washThe separated solvent phase was washed with brine
  6. dry with materialdried (MgSO4)
  7. customOn evaporation an oil
  8. customwas obtained
  9. customused without further purification

出典と根拠

ORDレコード
ord-c860e9ab15ed44159a48e3e704908253
出典データセット
uspto-grants-2008_04
特許番号
US07358376B2

関連ノート

読み込み中…