HRID6423

反应详情

EQUATION

反应方程式

HRID 6423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

ADAC, 2 (11.8 mg, 20 umol), was suspended in 0.5 ml DMF and treated with 4-isothiocyanato-TEMPO (2,2,6,6,-tetramethyl-1-piperidinyloxy, free radical (7 mg, Aldrich). After 1 hour 1.5 ml water was added to the solution, and the precipitate was collected, washed with a minimum of MeOH and ether, and recrystallized from DMF/ether/petroleum ether, to give a product which was homogeneous by thin layer chromatography and gave proton NMR and ESR spectra consistent with the structure. Yield 8.3 mg (51%). Cf-MS peak at 758 (m+1-MeO) and 626 (m+1 -ribose). IR shows a peak at 1580 cm-1, characteristic of a thiourea carbonyl stretch.

WORKUP

后处理

  1. customthe precipitate was collected
  2. washwashed with a minimum of MeOH and ether
  3. customrecrystallized from DMF/ether/petroleum ether
  4. customto give a product which
  5. customgave proton NMR and ESR spectra consistent with the structure