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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Morpholine → N-Cyclopropyl-6-(morpholin-4-yl)-4-propyl-1,3,5-triazin-2(1H)-imine

HRID 256707
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HRID 256707 반응식
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.Cl[C:8]1[N:13]=[C:12]([NH:14][CH:15]2[CH2:17][CH2:16]2)[N:11]=[C:10]([CH2:18][CH2:19][CH3:20])[N:9]=1>O1CCOCC1>[CH:15]1([NH:14][C:12]2[N:13]=[C:8]([N:1]3[CH2:6][CH2:5][O:4][CH2:3][CH2:2]3)[N:9]=[C:10]([CH2:18][CH2:19][CH3:20])[N:11]=2)[CH2:17][CH2:16]1
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참가 물질

4

반응물 2

HCID 8083MorpholineHCID 18965210HCID 18965210, 화합물

생성물 1

HCID 192460N-Cyclopropyl-6-(morpholin-4-yl)-4-propyl-1,3,5-triazin-2(1H)-imine수율 85%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

45 ml (0.45 mole) of morpholine dissolved in 200 ml of dioxane are added to a solution containing 43 g (0.163 mole) of 2-chloro-4-cyclopropylamino-6-n-propyl-1,3,5-triazine in 300 ml of dioxane, while maintaining the mixture at room temperature. After the addition, the mixture is heated under reflux for one to two hours. The reaction mixture is then allowed to return to room temperature and the precipitate is filtered off. The filtrate is concentrated and the residue is redissolved in dichloromethane. The solution is washed with water. The organic phase is separated off and dried over sodium sulfate. The solvent is evaporated under reduced pressure. The residue is purified by chromatography on silica (eluent: 98.5:1.5 (v/v) dichloromethane-ethanol) and the product is finally recrystallized from diethyl ether. 36.2 g of 2-cyclopropylamino-4-morpholino-6-n-propyl-1,3,5-triazine are obtained. Yield: 85%. M.P.: 104° C.

후처리

  1. additionare added to a solution
  2. additionAfter the addition
  3. temperaturethe mixture is heated
  4. temperatureunder reflux for one to two hours
  5. customto return to room temperature
  6. filtrationthe precipitate is filtered off
  7. concentrationThe filtrate is concentrated
  8. dissolutionthe residue is redissolved in dichloromethane
  9. washThe solution is washed with water
  10. customThe organic phase is separated off
  11. dry with materialdried over sodium sulfate
  12. customThe solvent is evaporated under reduced pressure
  13. customThe residue is purified by chromatography on silica (eluent: 98.5:1.5 (v/v) dichloromethane-ethanol)
  14. customthe product is finally recrystallized from diethyl ether

출처 및 근거

ORD 기록
ord-50096cab099648d1a08db906667096b3
출처 데이터셋
uspto-grants-1993_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05258513

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