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

HRID 647983ノート

反応式

HRID 647983 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1f60322c4f564679a042f179d6b57ab8
出典データセット
uspto-grants-1983_10
特許番号
US04410530

反応ノート

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