関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| 反応物 | Cyclamate | HCID 7533 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | Cyclohexylsulfamyl chloride | HCID 12914615 | 58% |
反応手順
A solution of 15 parts of dimethylcarbamic acid chloride in 310 parts of 1,2-dichloroethane is saturated with 30 parts of phosgene at 25° C and 89.5 parts of cyclohexylsulfamic acid are then added. The reaction mixture is heated to 83° C whilst continuing to introduce phosgene. In total, 330 parts of phosgene are introduced in the course of 13 hours. After removing the solvent and the dimethylcarbamic acid chloride under reduced pressure, the residue is distilled, and 57 parts (58% of theory) of cyclohexylsulfamic acid chloride of boiling point 208°-127° C/0.1 mm Hg and melting point 42°-44° C are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04101571 |
|---|
| 出典データセット | uspto-grants-1978_07 |
|---|
| ORD ID | ord-bd6bdfb9311641829d0d03b08693b735 |
|---|
| 出典メモ | uspto-grants-1978_07 |
|---|
