Ethylamine → 2,4-Diamino-6-ethylamino-1,3,5-triazine

HRID 365706ノート

反応式

HRID 365706 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4](Cl)[N:3]=1.[CH2:10]([NH2:12])[CH3:11].O1CCOCC1.[OH-].[Na+]>O>[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([NH:12][CH2:10][CH3:11])[N:3]=1

参加物

6

反応物 4

HCID 6341EthylamineHCID 14798Sodium HydroxideHCID 188311,3,5-Triazine-2,4-diamine, 6-chloro-HCID 312751,4-Dioxane

生成物 1

HCID 218192,4-Diamino-6-ethylamino-1,3,5-triazine収率 75%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixed solution of 14.5 g (0.1 mol) of 2,4-diamino-6-chloro-1,3,5-triazine prepared in Reference Example 1, 12.8 g (0.2 mol) of aqueous ethylamine solution (70%), 20 mL of water, and 50 mL of 1,4-dioxane was warmed with stirring and allowed to react at a reflux temperature for 4 hours. Thereafter, a solution of 4.0 g (0.1 mol) of sodium hydroxide in 15 mL of water was dropwise added thereto over 1 hour while maintaining the reflux state. After cooling the reaction mixture, the solvent and excess ethylamine were distilled off under reduced pressure, 30 mL each of methanol and acetonitrile were added, and the unnecessary salts were filtered. To the residue obtained by distilling off the solvent from the filtered solution were added 5 mL of methanol and 40 mL of acetone to precipitate crystals, which were collected by filtration, washed with 10 mL of acetone, and dried to obtain 11.5 g (yield 75%) of the titled compound. Melting point: 171° C.

後処理

  1. temperaturewas warmed
  2. customto react at a reflux temperature for 4 hours
  3. temperatureover 1 hour while maintaining the reflux state
  4. temperatureAfter cooling the reaction mixture
  5. distillationthe solvent and excess ethylamine were distilled off under reduced pressure, 30 mL each of methanol and acetonitrile
  6. additionwere added
  7. filtrationthe unnecessary salts were filtered
  8. customTo the residue obtained
  9. distillationby distilling off the solvent from the filtered solution
  10. additionwere added 5 mL of methanol and 40 mL of acetone
  11. customto precipitate crystals, which
  12. filtrationwere collected by filtration
  13. washwashed with 10 mL of acetone
  14. customdried

出典と根拠

ORDレコード
ord-d7db399304224acc9d4cc3d1de7f5649
出典データセット
uspto-grants-2000_10
特許番号
US06127538

反応ノート

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