反应详情

1,4,5,6-Tetrahydro-5-methoxycarbonylpyrimidine hydrochloride (I.49 g, 8.3 mmol), 1,8 diazabicyclo [5.4.0] undec-7ene, (hereinafter diazabicycloundecene and/or DBU), (2.5 mL, 16.6 mmol), and tritylchloride (2.32 g, 8.3 mmol) were suspended in anhydrous DMF (20 ml) with stirring under nitrogen at room temperature. After 18 hours stirring the suspension was evaporated in vacuo and the residue chromatographed (silica, chloroform/methanol, 9:1) to yield 2.28 g (rf=0.15, 71%) white crystalline solid identified by 300 MHz nmr and ms m/z=384.

1. stirringAfter 18 hours stirring the suspension
2. customwas evaporated in vacuo
3. customthe residue chromatographed (silica, chloroform/methanol, 9:1)
4. customto yield 2.28 g (rf=0.15, 71%) white crystalline solid