反应 #1914875

ord-b628f74a68624ca08b46c92469beeb03

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to come to room temperature
  2. 2
    workup.WAITleft
  3. 3
    浓缩the mixture was concentrated to dryness by rotary evaporation

实验过程

NaH (60% oil suspension containing 51 mg, 2.0 mmol) was added to a stirred solution of phenoxazine (147 mg, 0.784 mmol) in dry THF (10 mL) at 0° C. under N2. After 10 min. 2,4-diamino-6-bromomethylpteridine hydrobromide (100 mg, 0.392 mmol) was added and the reaction mixture was allowed to come to room temperature and left to stir for 2 days. The excess NaH was decomposed with MeOH (1 mL), and the mixture was concentrated to dryness by rotary evaporation. Flash chromatography on silica gel yielded the title compound, N-[(2,4-diaminopteridin-6-yl)methyl]phenoxazine, as a brown solid; yield 47 mg (34%); mp >250° C. dec. Anal. Calcd. for C19H15N7O0.4H2O: C, 62.60; H, 4.37. Found: C, 62.84; H, 4.10.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07056911B1uspto-grants-2006_06