Acetonitrile → HCID 59264606, 화합물

HRID 573477노트

반응식

HRID 573477 반응식
Br[C:2]([CH3:8])([CH3:7])[C:3]([O:5][CH3:6])=[O:4].O.Cl.[NH:11]1[CH2:16][CH2:15][C:14](=[O:17])[CH2:13][CH2:12]1.C(#N)C.C(=O)([O-])[O-].[K+].[K+]>C(OCC)C>[CH3:7][C:2]([N:11]1[CH2:16][CH2:15][C:14](=[O:17])[CH2:13][CH2:12]1)([CH3:8])[C:3]([O:5][CH3:6])=[O:4]

참가 물질

6

반응물 4

HCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 90097Methyl 2-bromo-2-methylpropionateHCID 2723901Piperonylamine

생성물 1

HCID 59264606HCID 59264606, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of methyl 2-bromo-2-methylpropanoate (80.87 ml, 5 equiv), 4-piperidone hydrochloride monohydrate (19.6 g, 1 equiv), acetonitrile (200 ml) and potassium carbonate (69.1 g, 4 equiv) was heated at reflux under nitrogen with mechanical stirring for 17.5 h then cooled in an ice bath before adding diethyl ether (100 ml). Filtration through celite followed by flash chromatography (silica, 10-50% ethyl acetate in hexane) and evaporation of the product fractions gave the desired product as a yellow oil (14.28 g).

후처리

  1. temperaturewas heated
  2. temperatureat reflux under nitrogen
  3. temperaturethen cooled in an ice bath
  4. filtrationFiltration through celite
  5. customfollowed by flash chromatography (silica, 10-50% ethyl acetate in hexane) and evaporation of the product fractions

출처 및 근거

ORD 기록
ord-474d69b0b65b4fc499a256a8e1ea85b3
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029383B2

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