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Diethylamine → HCID 10198815, 화합물

HRID 479098
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HRID 479098 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.[CH2:15]([NH:17][CH2:18][CH3:19])[CH3:16]>C(O)C>[CH2:15]([N:17]([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)[CH2:18][CH3:19])[CH3:16]
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참가 물질

4

반응물 2

HCID 8021DiethylamineHCID 11390207HCID 11390207, 화합물

생성물 1

HCID 10198815HCID 10198815, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
100 °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 diethylamine (2.00 mL) in absolute ethanol (2.0 mL) was heated to 100° C. in a sealed tube for 5 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 65 mg of yellow colored 3-Diethylaminomethyl-pyrimido[5,4-e][1,2,4]triazine-5,7-diamine 4 as the trifluoroacetate salt.

후처리

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

출처 및 근거

ORD 기록
ord-f33ec443377842e083b6a2d63c1e56bc
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06642381B2

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