Sodium Hydroxide → N-Octadecyl-1,3,5-triazine-2,4,6-triamine

HRID 365708

반응식

HRID 365708 반응식
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4](Cl)[N:3]=1.O1CCOCC1.[CH2:16]([NH2:34])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33].[OH-].[Na+]>O>[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([NH:34][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33])[N:3]=1

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 15793OctadecylamineHCID 188311,3,5-Triazine-2,4-diamine, 6-chloro-HCID 312751,4-Dioxane

생성물 1

HCID 89073N-Octadecyl-1,3,5-triazine-2,4,6-triamine수율 91%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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, 60 mL of water, 60 mL of 1,4-dioxane, and 26.9 g (0.1 mol) of octadecylamine was warmed with stirring and allowed to react at a reflux temperature for 3 hours. Further, an aqueous solution of 4.0 g (0.1 mol) of sodium hydroxide in 20 mL of water was dropwise added thereto over 1 hour and the mixture was allowed to react for additional 2 hours. After cooling the reaction mixture, the solvent was distilled off under reduced pressure, and 100 mL of water and 100 mL of toluene were added to extract the product in the organic layer. After washing the organic layer with water sufficiently, the solvent was distilled off from the organic layer to obtain 34.4 g (yield 91%) of the titled compound. Melting point: 91° C.

후처리

  1. temperaturewas warmed
  2. customto react at a reflux temperature for 3 hours
  3. customto react for additional 2 hours
  4. temperatureAfter cooling the reaction mixture
  5. distillationthe solvent was distilled off under reduced pressure, and 100 mL of water and 100 mL of toluene
  6. additionwere added
  7. extractionto extract the product in the organic layer
  8. washAfter washing the organic layer with water sufficiently
  9. distillationthe solvent was distilled off from the organic layer

출처 및 근거

ORD 기록
ord-079ca171ee43460fa7dfd678ad3dff7c
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06127538

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