تفاعل #2275684

معادلة التفاعل

Acetic acid [(3,5-bis-chlorocarbonyl-2,4,6-triiodo-phenyl)-methyl-carbamoyl]-methyl ester

propanediol

DMA

methanol

→

acetic acid ({3-chlorocarbonyl-5-[(2,3-dihydroxy-propyl)-methyl-carbamoyl]-2,4,6-triiodo-phenyl}-methyl-carbamoyl)-methyl ester

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   غسيلwashed with ice water/brine (50:50, 20 ml×3)
2. 2
   أخرىThe organics were collected
3. 3
   تجفيفdried over MgSO4
4. 4
   ترشيحfiltered
5. 5
   أخرىevaporated to dryness
6. 6
   أخرىThe product was purified by silica column chromatography
7. 7
   غسيلeluting with DCM

الإجراء التجريبي

Acetic acid [(3,5-bis-chlorocarbonyl-2,4,6-triiodo-phenyl)-methyl-carbamoyl]-methyl ester (16.25 g, 22.9 mmol) and 3-methylamino-1,2,-propanediol (4.42 ml, 45.8 mmol) were stirred in DMA (80 ml) for 72 hours at room temperature. The mixture was diluted with ethyl acetate (150 ml) and washed with ice water/brine (50:50, 20 ml×3). The organics were collected, dried over MgSO4, filtered and evaporated to dryness. The product was purified by silica column chromatography eluting with DCM: methanol to give acetic acid ({3-chlorocarbonyl-5-[(2,3-dihydroxy-propyl)-methyl-carbamoyl]-2,4,6-triiodo-phenyl}-methyl-carbamoyl)-methyl ester (5.42 g, 6.96 mmol).

المصدر