Cyclopropylamine → N~2~,N~4~,N~6~-Tricyclopropyl-1,3,5-triazine-2,4,6-triamine

HRID 1448778ノート

反応式

HRID 1448778 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][CH:9]2[CH2:11][CH2:10]2)[N:5]=[C:4]([NH:12][CH:13]2[CH2:15][CH2:14]2)[N:3]=1.[CH:16]1([NH2:19])[CH2:18][CH2:17]1>O1CCOCC1>[CH:16]1([NH:19][C:2]2[N:7]=[C:6]([NH:8][CH:9]3[CH2:11][CH2:10]3)[N:5]=[C:4]([NH:12][CH:13]3[CH2:15][CH2:14]3)[N:3]=2)[CH2:18][CH2:17]1

参加物

4

反応物 2

HCID 69828CyclopropylamineHCID 6430808HCID 6430808、化合物

生成物 1

HCID 57290175N~2~,N~4~,N~6~-Tricyclopropyl-1,3,5-triazine-2,4,6-triamine

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
140 °C

実験手順

A mixture of 20 g of 2-chloro-4,6-bis-cyclopropylamino-s-triazine, 10.1 g of cyclopropylamine and 80 ml of dioxan is heated at 140° C. in an autoclave for 22 hours. The reaction mixture is concentrated in vacuo to half its volume and 300 ml of water are added. The mixture is extracted with ethyl acetate, the product phase is dried over sodium sulfate and the solvents are removed in vacuo. The residue is recrystallised from dioxan/petroleum ether; melting point 75°-77° C.

後処理

  1. concentrationThe reaction mixture is concentrated in vacuo to half its volume and 300 ml of water
  2. additionare added
  3. extractionThe mixture is extracted with ethyl acetate
  4. dry with materialthe product phase is dried over sodium sulfate
  5. customthe solvents are removed in vacuo
  6. customThe residue is recrystallised from dioxan/petroleum ether

出典と根拠

ORDレコード
ord-be9ceb9e994d444193d71bfb373bd838
出典データセット
uspto-grants-1980_02
特許番号
US04187305

反応ノート

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