참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | DTPA dianhydride | HCID 100825 | — |
| 반응물 | Ethyl 11-aminoundecanoate | HCID 13192100 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3,6-Bis(carboxymethyl)-9-(10-carbethoxydecylcarbamoylmethyl)-3,6,9-triazaundecanedioic acid | HCID 10210919 | — |
반응 단계
17.85 g (50 mmol) of 1.5-bis(2,6-dioxomorpholino)-3-carboxymethyl-3-azapentane is stirred in 200 ml of dimethylformamide and mixed with 9 ml (50 mmol) of water. The solution is heated for 3 hours to 70° C., cooled off to 0° C. and 36.07 ml (260 mmol) of triethylamine and 10.8 g (50 mmol) of 11-aminoundecanoic acid ethyl ester are added. After stirring overnight at room temperature, the solution is evaporated to dryness in a vacuum. The residue is taken up in 100 ml of water and the solution is mixed by drops with concentrated hydrochloric acid until permanent cloudiness. After stirring overnight in the ice bath, the finely crystalline precipitate is suctioned off, washed with water and dried in a vacuum at 50° C. 14.9 g (65% of theory) of the title compound is obtained as a white powder with melting point 155-157° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06565830B1 |
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| 출처 데이터셋 | uspto-grants-2003_05 |
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| ORD ID | ord-a595cd5bdf54430e8c1443416e011d35 |
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| 출처 메모 | uspto-grants-2003_05 |
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