関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Chloroacetamide | HCID 6580 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | methyl N-(2-chloroacetyl)carbamate | HCID 518783 | — |
反応手順
A suspension of 2-chloroacetamide (122.6 g, 1.31 mol) in 300 ml of 1,2-dichloroethane is cooled to 0° C. and treated with oxalyl chloride (200 g, 1.57 mol). The reaction mixture is heated at reflux for 4 hours. After cooling to 5° C., 68 ml of MeOH is added dropwise while keeping the internal temperature below 15° C. with external cooling. After addition is complete, the product is separated by filtration and washed with CH2Cl2 and Et2O. Recrystallization from CH2Cl2 yields methyl(chloroacetyl)carbamate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04221796 |
|---|
| 出典データセット | uspto-grants-1980_09 |
|---|
| ORD ID | ord-93e933a150fd4dfdad3e601d64c283ad |
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| 出典メモ | uspto-grants-1980_09 |
|---|
