関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Dihydroxyacetone | HCID 670 | — |
| 反応物 | Iminoethyl methoxyacetate hydrochloride | HCID 57478929 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178494684 | HCID 178494684 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06710055B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-7e21ca4540c6429c96d42769f9678dad |
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| 出典メモ | uspto-grants-2004_03 |
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