反応 #164022

反応方程式

(S)-1-chloro-1-oxopropan-2-yl acetate

5-amino-2,4,6-triiodoisophthalic acid

→

(S)-5-(2-acetoxypropanamido)-2,4,6-triiodoisophthalic acid

収率 81.0%

溶媒

DMA

反応条件

後処理

1. 1
   温度heating
2. 2
   その他was removed
3. 3
   workup.STIRRINGthe mixture was stirred for about 14 hours at room temperature
4. 4
   workup.ADDITIONThe reaction mixture was added slowly over water (500 ml)
5. 5
   workup.STIRRINGwith strong stirring at a temperature between 22° C. and 30° C
6. 6
   workup.ADDITIONAfter addition 300 ml of water
7. 7
   workup.ADDITIONwere added to the suspension
8. 8
   workup.STIRRINGThe suspension was stirred for 5 further hours at about 22° C. after which the white solid
9. 9
   ろ過was filtered
10. 10
    洗浄washed with water
11. 11
    温度previously cooled at about 5° C. twice (30 ml each time)
12. 12
    その他The product was dried in a vacuum oven at about 5.0° C.

実験手順

(S)-1-chloro-1-oxopropan-2-yl acetate (37.4 ml, 295.4 mmol) was added slowly to a suspension of 5-amino-2,4,6-triiodoisophthalic acid (50.0 g, 89.5 mmol) in DMA (100 ml) at a temperature of between 25° C. and 29° C. The resulting mixture was heated to about 50° C. and stirred at this temperature for about 8 hours after which heating was removed and the mixture was stirred for about 14 hours at room temperature. The reaction mixture was added slowly over water (500 ml) with strong stirring at a temperature between 22° C. and 30° C. After addition 300 ml of water were added to the suspension. The suspension was stirred for 5 further hours at about 22° C. after which the white solid was filtered and washed with water previously cooled at about 5° C. twice (30 ml each time). The product was dried in a vacuum oven at about 5.0° C. to yield (S)-5-(2-acetoxypropanamido)-2,4,6-triiodoisophthalic acid (48.8 g, 72.5 mmol).

出典