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

HRID 900433

반응식

HRID 900433 반응식
[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]

참가 물질

9

반응물 4

HCID 313Hydrochloric AcidHCID 79752-MethylpyridineHCID 31374DimethylacetamideHCID 178418339Butyllithium

생성물 1

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

시약·촉매·용매 4

HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8058Hexane용매HCID 8857Ethyl Acetate용매

반응 조건

온도
-75 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c860e9ab15ed44159a48e3e704908253
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07358376B2

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