Реакция #62731

Уравнение реакции

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

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title compound

Выход 37.0%

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

Выход 37.0%

Растворители

N,N-diethylaniline

Условия реакции

Обработка

1. 1
   ФильтрацияThe hot solution was filtered
2. 2
   Другоеto remove dark tarry material
3. 3
   ТемператураThe filtrate was cooled
4. 4
   workup.ADDITIONdiluted with hexanes (200 mL)
5. 5
   ДругоеThe precipitate (3.8 g) was recrystallized from ethanol

Методика

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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