Methylamine → 2-Methylamino-4-difluoromethoxy-6-methylpyrimidine

HRID 1719787ノート

反応式

HRID 1719787 の反応式
[CH3:1][NH2:2].CS([C:7]1[N:12]=[C:11]([O:13][CH:14]([F:16])[F:15])[CH:10]=[C:9]([CH3:17])[N:8]=1)(=O)=O>C(Cl)Cl>[CH3:1][NH:2][C:7]1[N:12]=[C:11]([O:13][CH:14]([F:16])[F:15])[CH:10]=[C:9]([CH3:17])[N:8]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 134918212-Methylsulfonyl-4-difluoromethoxy-6-methylpyrimidine

生成物 1

HCID 134918222-Methylamino-4-difluoromethoxy-6-methylpyrimidine収率 74%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

30 ml of a 40% aqueous methylamine solution are added, at a temperature of between 20° and 25° C., to 2.2 g (0.009 mol) of 2-methylsulfonyl-4-difluoromethoxy-6-methylpyrimidine. The mixture warms up to a temperature of 60° C. The reaction mixture is subsequently stirred for half an hour at the same temperature; it is then cooled and 50 ml of methylene chloride are added. The organic phase is separated, dried over sodium sulfate and concentrated by evaporation. Crystallisation of the residue from a methylene chloride/petroleum ether mixture yields 1.4 g (74% of theory) of 2-methylamino-4-difluoromethoxy-6 -methylpyrimidine, m.p. 129.5°-131° C.

後処理

  1. customwarms up to a temperature of 60° C
  2. temperatureit is then cooled
  3. customThe organic phase is separated
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated by evaporation
  6. customCrystallisation of the residue from a methylene chloride/petroleum ether mixture

出典と根拠

ORDレコード
ord-4edbee7928b040dba5cfc47cfc7e2dee
出典データセット
uspto-grants-1985_09
特許番号
US04542216

反応ノート

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