참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Dihydroxyacetone | HCID 670 | — |
| 반응물 | Iminoethyl methoxyacetate hydrochloride | HCID 57478929 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 178494684 | HCID 178494684 | — |
반응 단계
A mixture of 30.6 g (0.20 mol) of iminoethyl methoxyacetate hydrochloride, 18 g (0.20 mol) of 1,3-dihydroxyacetone and 200 mL of liquid ammonia was heated to 68° C. for 3 hours in a stirred autoclave at a pressure of 27 bar (analogously to: P. Dziuron et al., Arch. Pharm. 307, 1974, p.470). Then the ammonia was eliminated and 200 mL of methylene chloride were added. The white precipitate formed was filtered off and washed with methylene chloride. The filtrate was evaporated down and the residue obtained was purified by chromatography (aluminium oxide; methylene chloride/ethanol=90:10 to 85:15). Yield: 26.7 g (94% of theory), C6H10N2O2 (142.20); Rf value: 0.43 (silica gel; methylene chloride/ethanol=9:1); mass spectrum: (M)+=142.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06710055B2 |
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| 출처 데이터셋 | uspto-grants-2004_03 |
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| ORD ID | ord-7e21ca4540c6429c96d42769f9678dad |
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| 출처 메모 | uspto-grants-2004_03 |
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