Sodium Hydroxide → 1211518-11-4

HRID 891219ノート

反応式

HRID 891219 の反応式
[Cl:1]Cl.[NH2:3][C:4]1[N:9]=[C:8](SC)[N:7]=[C:6]([C:12]([F:15])([F:14])[F:13])[N:5]=1.[OH-].[Na+]>C(O)(=O)C>[NH2:3][C:4]1[N:9]=[C:8]([Cl:1])[N:7]=[C:6]([C:12]([F:15])([F:14])[F:13])[N:5]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24526ChlorineHCID 22244968HCID 22244968、化合物

生成物 1

HCID 222449641211518-11-4収率 60%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
20 °C

実験手順

Chlorine gas was passed into a solution of 21 g of 2-amino-4-methylthio-6-trifluoromethyl-1,3,5-triazine in 0.2 l glacial acetic acid at 20 to 25° C. (15 min). The reaction mixture was stirred for 30 min at approx. 20° C., sprayed for 1 hour with nitrogen gas at room temperature, poured into 1 l of ice-cold aqueous solution of 70 g of sodium hydroxide and stirred for 5 min. After extraction with ethyl acetate, the organic phase was washed with water and dried over magnesium sulfate, and the solvent was removed in vacuo. The crude product was purified by stirring in heptane. After filtration with suction and drying, 12 g (60%) of 2-amino-4-chloro-6-trifluoromethyl-1,3,5-triazine were obtained as a white powder (m.p. 109° C.); 1H NMR (CDCl3): δ=6.4 (s br., 2H).

後処理

  1. custom(15 min)
  2. waitsprayed for 1 hour with nitrogen gas at room temperature
  3. stirringstirred for 5 min
  4. extractionAfter extraction with ethyl acetate
  5. washthe organic phase was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customthe solvent was removed in vacuo
  8. customThe crude product was purified
  9. stirringby stirring in heptane
  10. filtrationAfter filtration with suction
  11. customdrying

出典と根拠

ORDレコード
ord-3a9fbc8fc9d94692bfac57c74f3a0eed
出典データセット
uspto-grants-2006_02
特許番号
US07002011B1

反応ノート

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