Cyanuric chloride → 2-Chloro-4,6-bis-(2,2,6,6-tetramethyl-4-piperidyl-butylamino)-1,3,5-triazine

HRID 484935

反応式

HRID 484935 の反応式
[N:1]1[C:8](Cl)=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].[CH2:10]([NH:14][CH:15]1[CH2:20][C:19]([CH3:22])([CH3:21])[NH:18][C:17]([CH3:24])([CH3:23])[CH2:16]1)[CH2:11][CH2:12][CH3:13]>O1CCOCC1>[Cl:3][C:2]1[N:1]=[C:8]([N:14]([CH2:10][CH2:11][CH2:12][CH3:13])[CH:15]2[CH2:16][C:17]([CH3:23])([CH3:24])[NH:18][C:19]([CH3:22])([CH3:21])[CH2:20]2)[N:7]=[C:5]([N:14]([CH:15]2[CH2:16][C:17]([CH3:24])([CH3:23])[NH:18][C:19]([CH3:21])([CH3:22])[CH2:20]2)[CH2:10][CH2:11][CH2:12][CH3:13])[N:4]=1

参加物

4

反応物 2

HCID 7954Cyanuric chlorideHCID 118285n-Butyl-2,2,6,6-tetramethyl-4-piperidinamine

生成物 1

HCID 111142202-Chloro-4,6-bis-(2,2,6,6-tetramethyl-4-piperidyl-butylamino)-1,3,5-triazine

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of 18.4 g of cyanuric chloride in 200 ml of dioxane was added dropwise, with stirring, a solution of 43.6 g of 4-butylamino-2,2,6,6-tetramethylpiperidine in 100 ml of dioxane at 20°-25° C. The mixture was stirred at the same temperature for 2 hours, after which it was stirred at 60°-70° C. for 2 hours. At the end of this time, the dioxane was distilled off and the residue was poured into a 10% aqueous solution of potassium carbonate and extracted with ethyl acetate. The extract was dried over anhydrous potassium carbonate, and then the ethyl acetate was distilled off. The resulting oil was purified by column chromatography through silica gel, eluted with a 20:1:1 by volume mixture of ethyl acetate, ethanol and triethylamine, to give the title compound in the form of crystals melting at 40°-42° C.

後処理

  1. customat 20°-25° C
  2. stirringThe mixture was stirred at the same temperature for 2 hours
  3. stirringafter which it was stirred at 60°-70° C. for 2 hours
  4. distillationAt the end of this time, the dioxane was distilled off
  5. additionthe residue was poured into a 10% aqueous solution of potassium carbonate
  6. extractionextracted with ethyl acetate
  7. dry with materialThe extract was dried over anhydrous potassium carbonate
  8. distillationthe ethyl acetate was distilled off
  9. customThe resulting oil was purified by column chromatography through silica gel
  10. washeluted with a 20:1:1 by volume mixture of ethyl acetate, ethanol and triethylamine

出典と根拠

ORDレコード
ord-9da1fe9f6da34451a8adbe6533a12bd3
出典データセット
uspto-grants-1985_08
特許番号
US04533688

関連ノート

読み込み中…