関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 5-Amino-2,4,6-triiodo-1,3-benzenedicarboxylic acid | HCID 3015783 | — |
| 反応物 | (1S)-2-Chloro-1-methyl-2-oxoethyl acetate | HCID 11094804 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | (S)-(-)-5-[(2-Acetoxypropanoyl)amino]-2,4,6-triiodoisophthalic Acid | HCID 15817302 | 57.5% |
反応手順
(S)-1-chloro-1-oxopropan-2-yl acetate (0.75 ml, 5.91 mmol) was added drop-wise to a solution of 5-amino-2,4,6-triiodoisophthalic acid (1.0 g, 1.79 mmol) in DMA (5 ml). The resulting mixture was stirred at about 50° C. for 5 hours and 20 minutes. 80 ml of water was added to the reaction mixture at room temperature after which the suspension formed was cooled to a temperature between 0° C. and 5° C. and stirred for 25 minutes at this temperature. The suspension was filtered and the solid washed with water. The product was dried in a vacuum oven at 40° C. to yield (S)-5-(2-acetoxypropanamido)-2,4,6-triiodoisophthalic acid (0.695 g, 1.03 mmol). The MS, 1H-NMR and 13C-NMR data are consistent with the structure for (S)-5-(2-acetoxypropanamido)-2,4,6-triiodoisophthalic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08835672B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-ab0b12a16a294dd3a941a09e08b3714b |
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| 出典メモ | uspto-grants-2014_09 |
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