反応 #65070

反応方程式

1-Chloro-1-phenylmethyl phenyl carbonate

potassium 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzene carboxylate

sodium iodide

→

1-(Phenyloxycarbonyloxy)-1-phenylmethyl 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate

溶媒

DMF

反応条件

後処理

1. 1
   その他at room temperature for 18 hours the solvent was removed at reduced pressure
2. 2
   洗浄washed four times with a saturated sodium hydrogen carbonate solution
3. 3
   乾燥After drying with magnesium sulfate the solution
4. 4
   その他was evaporated to dryness

実験手順

1-Chloro-1-phenylmethyl phenyl carbonate (0.63 g, 2.4 mmol) was added at room temperature to a solution of potassium 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzene carboxylate (1.44 g, 2.2 mmol) and sodium iodide (0.034 g, 0.23 mmol) in dry DMF (12 ml). After stir ring at 60° C. for 2 hours and at room temperature for 18 hours the solvent was removed at reduced pressure. The residue was suspended in chloroform (20 ml) and washed four times with a saturated sodium hydrogen carbonate solution and finally twice with water. After drying with magnesium sulfate the solution was evaporated to dryness. Yield: 0.90 g. Purity by HPLC: 96.6% 1H-NMR(DMSO-d6): delta=1.67 (NCH3COCH3 ); 2.05 (NHCOCH3); 2.96 (NCH3); 7.29-7.54 (phenyl); 7.71 (CH); 10.13 ppm (NH). FAB/MS: 854 (M+).

出典