反応 #62731

反応方程式

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

→

title compound

収率 37.0%

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

収率 37.0%

溶媒

N,N-diethylaniline

反応条件

後処理

1. 1
   ろ過The hot solution was filtered
2. 2
   その他to remove dark tarry material
3. 3
   温度The filtrate was cooled
4. 4
   workup.ADDITIONdiluted with hexanes (200 mL)
5. 5
   その他The precipitate (3.8 g) was recrystallized from ethanol

実験手順

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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