반응 #62731

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2,4-diamino-5-[3,4-dimethoxy-5-(1-methyl-2-propynyloxy)benzyl]pyrimidine

→

title compound

수율 37.0%

2,4-Diamino-5-(7,8-dimethoxy-2-methyl-2H-1-benzopyran-5-ylmethyl)pyrimidin

수율 37.0%

용매

N,N-diethylaniline

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후처리

1. 1
   여과The hot solution was filtered
2. 2
   기타to remove dark tarry material
3. 3
   온도The filtrate was cooled
4. 4
   workup.ADDITIONdiluted with hexanes (200 mL)
5. 5
   기타The precipitate (3.8 g) was recrystallized from ethanol

실험 절차

A solution of 2,4-diamino-5-[3,4-dimethoxy-5-(1-methyl-2-propynyloxy)benzyl]pyrimidine (4.28 g, 13.0 mmol) in N,N-diethylaniline (200 mL) was refluxed under nitrogen for 0.5 hr. The hot solution was filtered to remove dark tarry material. The filtrate was cooled and diluted with hexanes (200 mL). The precipitate (3.8 g) was recrystallized from ethanol to give title compound as off-white powder (1.56 g, 37%); mp 219°-221° dec. Anal. Calcd for C17H20N4O3 : C, 62.18; H, 6.14; N, 17.06. Found: C, 61.91; H, 6.20; N, 16.93.

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