참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Triphosgene | HCID 94429 | — |
| 반응물 | Hydroxy ethylmaleimide | HCID 22337974 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 17973880 | HCID 17973880 | 154.9% |
반응 단계
Hydroxy ethylmaleimide (10.0 g, 70.1 mmol) was dissolved in a solution of methylene chloride (71 mL) and triethylamine (9.87 mL, 70.8 mmol) and cooled with an ice bath to 0° C. Triphosgene (3.504 g, 12 mmol) was added over a period of 4 hours and the resulting solution filtered. The supernatant was washed with 1N hydrochloric acid, 5% potassium carbonate solution and water. The solution was dried over magnesium sulfate and purified using activated carbon to yield white crystals (4.0 g, 18.5%). 1H-NMR (CDCl3, δ, ppm): 3.82 (4H, —NCH2—, t), 4.27 (2H, —CH2O—, t), 6.73 (2H, —CH═CH—, s). 13C-NMR (CDCl3, δ, ppm): 36.6 (2C, —NCH2—), 64.9 (2C, —CH2O—), 134.2 (2C, —CH═CH—), 154.5 (1C, C═O) 170.8 (2C, —NC═O).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06855745B2 |
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| 출처 데이터셋 | uspto-grants-2005_02 |
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| ORD ID | ord-5df5317e50ca472a840b558e494050c0 |
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| 출처 메모 | uspto-grants-2005_02 |
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