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ethyl N-carbonylcarbamate → ethyl N-diethoxyphosphorylcarbonylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | ethyl N-carbonylcarbamate | HCID 300166 | — |
| 反応物 | Diethylphosphite | HCID 3780918 | — |
| 触媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | ethyl N-diethoxyphosphorylcarbonylcarbamate | HCID 21415674 | — |
反応手順
To a solution of 11.0 parts of diethylphosphite in 175 parts of methylene chloride and 4 drops of triethyl amine was added 10.0 parts of ethoxycarbonyl isocyanate. The solution was refluxed for 3 hours. Removing the solvent under reduced pressure left 18.5 parts of colorless oil which partially crystallized. The crystals were washed with cyclohexane to give 7.3 parts of ethyl N-(diethylphosphonocarbonyl)carbamate, m.p. 75° -64° , The proton nmr spectrum was consistent with this structure (δNH = 10.0 ppm)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04043793 |
| 出典データセット | uspto-grants-1977_08 |
| ORD ID | ord-8df23a969ce244d9ab731cbc768b4fe2 |
| 出典メモ | uspto-grants-1977_08 |