Sodium Hydroxide → HCID 12040787、化合物

HRID 891218ノート

反応式

HRID 891218 の反応式
[Cl:1]Cl.[NH2:3][C:4]1[N:9]=[C:8](SC)[N:7]=[C:6]([CH:12]([F:14])[CH3:13])[N:5]=1.[OH-].[Na+]>C(O)(=O)C>[NH2:3][C:4]1[N:9]=[C:8]([Cl:1])[N:7]=[C:6]([CH:12]([F:14])[CH3:13])[N:5]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24526ChlorineHCID 222449654-(1-Fluoroethyl)-6-(methylthio)-1,3,5-triazin-2-amine

生成物 1

HCID 12040787HCID 12040787、化合物収率 70%

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 suspension of 38 g of 2-amino-4-methylthio-6-(1-fluoroethyl)-1,3,5-triazine in 0.25 l of glacial acetic acid (15 min) at 20 to 25° C. The reaction mixture was stirred for 30 min at approx. 20° C., sprayed for 1 hour with nitrogen gas at room temperature, poured into 1.25 l of ice-cold aqueous solution of 87 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, 25 g (70%) of 2-amino-4-chloro-6-(1-fluoroethyl)-1,3,5-triazine were obtained as a white powder (m.p. 131° C.); 1H NMR (CDCl3): δ=1.7 (dd, 3 H), 5.4 (dq, 1 H), 6.1 (s br., 1 H), 6.7 (s br., 1H).

後処理

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

出典と根拠

ORDレコード
ord-723b383e40c342508da3f2f11da2cb75
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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