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

HRID 1448778노트

반응식

HRID 1448778 반응식
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

참가 물질

4

반응물 2

HCID 69828CyclopropylamineHCID 6430808HCID 6430808, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
140 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-be9ceb9e994d444193d71bfb373bd838
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04187305

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