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Morpholine → HCID 12109539, 화합물

HRID 479101
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HRID 479101 반응식
Cl[CH2:2][C:3]1[N:4]=[N:5][C:6]2[C:7](=[C:9]([NH2:14])[N:10]=[C:11]([NH2:13])[N:12]=2)[N:8]=1.[NH:15]1[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1>>[N:15]1([CH2:2][C:3]2[N:4]=[N:5][C:6]3[C:7](=[C:9]([NH2:14])[N:10]=[C:11]([NH2:13])[N:12]=3)[N:8]=2)[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 8083MorpholineHCID 11390207HCID 11390207, 화합물

생성물 1

HCID 12109539HCID 12109539, 화합물

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온도
80 °C

실험 절차

A mixture of 3-Chloromethyl-pyrimido[5,4-e][1,2,4]triazine-5,7-diamine 3 (200 mg; 0.95 mmol) and 2.0 mL of morpholine were heated to 80° C. in a sealed tube for 7 h. The mixture was then allowed to cool to room temperature and concentrated in vacuo. The crude product was purified by reverse phase HPLC (Rainin C18, 0% CH3CN to 30% CH3CN gradient, CH3CN/H2O, 0.1% TFA) and the bright yellow fractions containing the product were lyophilized after removal of CH3CN in vacuo to give 261 mg of yellow colored 3-Morpholin-4-ylmethyl-pyrimido[5,4-e][1,2,4]triazine-5,7-diamine as the trifluoroacetate salt.

후처리

  1. temperatureto cool to room temperature
  2. concentrationconcentrated in vacuo
  • customThe crude product was purified by reverse phase HPLC (Rainin C18, 0% CH3CN to 30% CH3CN gradient, CH3CN/H2O, 0.1% TFA)
  • additionthe bright yellow fractions containing the product
  • customafter removal of CH3CN in vacuo
  • 출처 및 근거

    ORD 기록
    ord-f52ef5659c704d529557714b9e5572fd
    출처 데이터셋
    uspto-grants-2003_11
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06642381B2

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