反応 #65063

反応方程式

1-Chloroethyl phenyl carbonate

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

potassium iodide

→

1-(Phenyloxycarbonyloxy)ethyl 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-Chloroethyl phenyl carbonate (prepared according to Synthesis 1986, 627) (2.21 g, 11 mmol) was added at room temperature to a solution of potassium 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate (6.66 g, 10 mmol) and potassium iodide (0.17 g, 1 mmol) in dry DMF. After stirring at 50° C. for 6 hours and at room temperature for 4 days the solvent was removed at reduced pressure. The residue was suspended in chloroform (100 ml) and washed four times with a saturated sodium hydrogen carbonate solution and twice with water. After drying with magnesium sulfate the solution was evaporated to dryness. Yield: 7.3 g. Purity by HPLC: 98%. 1H-NMR (DMSO-d6): delta=1.68 (N(CH3)COCH3); 1.74 (CHCH3); 2.05 (NCOCH3); 2.97 (NCH3); 7.05 (CH); 7.25-7.52 (arom.); 10.14 ppm (NH).

出典