참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Carbamic acid, ethyl ester | HCID 5641 | — |
| 반응물 | 2,4-Diaminotoluene | HCID 7261 | — |
| 반응물 | Ethanol, reaction products with ammonia, distn. residues | HCID 22020343 | — |
| 생성물 | Diethyl toluene-2,4-dicarbamate | HCID 343975 | 64.1% |
반응 단계
122 g (1 mol) of 2,4-Diaminotoluene and 1782 g (20 mol) of ethyl carbamate are heated to 200° C. in the presence of 320 g of ethanol, with stirring, in a 5-liter stirrer autoclave, and 1300 ml of an ammonia/ethanol mixture are distilled off per hour. The autoclave is adjusted to a pressure of from 6 to 10 bar by means of a control valve and the ethanol concentration is kept constant by pumping in fresh ethanol. After a reaction time of 5 hours, the autoclave is left to cool down, emptied, and the alcohol is distilled at 40° to 90° C./90 mbar. The distillation residue (1224 g) is taken up with 1200 g of water at 95° C. and intensively stirred. 260 g of 2,4-bis-(ethoxycarbonylamino)-toluene precipitate after cooling of the solution to 40° C. and are filtered off. The 2,4-bis-(ethoxycarbonylamino)-toluene is again taken up with 300 g of boiling water, and reprecipitated at 40° C. 170.4 g (64.1% of theoretical) of 2,4-bis-(ethoxycarbonylamino)-toluene are obtained after drying over night in a drying cupboard at 90° C./100 mbar.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05399736 |
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| 출처 데이터셋 | uspto-grants-1995_03 |
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| ORD ID | ord-e3c433cda3634a79a4ee6e617280c635 |
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| 출처 메모 | uspto-grants-1995_03 |
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