Methylamine → 3-Pyridinecarboxamide, 5,6-dichloro-N-methyl-

HRID 1764347노트

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HRID 1764347 반응식
[Cl:1][C:2]1[C:3]([Cl:11])=[N:4][CH:5]=[C:6]([CH:10]=1)[C:7](Cl)=[O:8].[CH3:12][NH2:13]>C(Cl)(Cl)Cl.C(O)C>[Cl:11][C:3]1[C:2]([Cl:1])=[CH:10][C:6]([C:7]([NH:13][CH3:12])=[O:8])=[CH:5][N:4]=1

참가 물질

5

반응물 2

HCID 6329MethylamineHCID 27821565,6-dichloropyridine-3-carbonyl Chloride

생성물 1

HCID 204834083-Pyridinecarboxamide, 5,6-dichloro-N-methyl-

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6212Chloroform용매

실험 절차

A solution of 30 g of crude 5,6-dichloronicotinic acid chloride in 150 ml of chloroform is added dropwise to a solution of 50 g of methylamine in 250 ml of ethanol whilst stirring and cooling at 10°-15° C. The reaction mixture is stirred for a further 2 hours at 20°-30° C. and is then evaporated in vacuo. The evaporation residue is taken up in ethyl acetate and this solution is washed with 2 N sodium carbonate solution, dried over magnesium sulphate and evaporated. The residue is recrystallised from ethanol-ether. 2,3-Dichloro-5-methylaminocarbonyl-pyridine, thus obtained, melts at 134°-138° C.

후처리

  1. temperaturecooling at 10°-15° C
  2. stirringThe reaction mixture is stirred for a further 2 hours at 20°-30° C.
  3. customis then evaporated in vacuo
  4. washthis solution is washed with 2 N sodium carbonate solution
  5. dry with materialdried over magnesium sulphate
  6. customevaporated
  7. customThe residue is recrystallised from ethanol-ether

출처 및 근거

ORD 기록
ord-5b1164b6b1a94394bf29a3f155f21372
출처 데이터셋
uspto-grants-1978_09
특허 번호
US04115575

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