참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | N-methylhydroxylamine hydrochloride | HCID 77906 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 반응물 | N-(2-Methylprop-2-enyl)-N-(2-oxoethyl)-urethane | HCID 15069992 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | Ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate | HCID 15070010 | — |
반응 단계
21.7 g of 30% strength sodium methylate solution are added dropwise to 10 g (0.12 mol) of N-methylhydroxylamine hydrochloride in 26 ml of methanol. The sodium chloride is filtered off with suction and washed with 8 ml of methanol and 80 ml of toluene. This solution is added dropwise to 19.2 g (0.11 mol) of N-(2-methyl-prop-2-enyl)-N-(2-oxoethyl)-urethane, which is heated under reflux in 160 ml of toluene using a water separator. The mixture is heated under reflux overnight, the product is extracted with 160 ml of 10% strength hydrochloric acid and the hydrochloric acid solution is rendered alkaline with potassium carbonate and extracted with six portions, of 200 ml of CHCl3. The extracts are dried over K2CO3 and concentrated and the residue is distilled.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05416096 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-7020e83ef5a14745ace0469bb96f35b9 |
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| 출처 메모 | uspto-grants-1995_05 |
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