化工社化工社 化学情報印刷レポート · 研究参考用
Thiophosgene → 2,4-Dichloro-6-fluoro-7-isothiocyanatobenzothiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiophosgene | HCID 10040 | — |
| 反応物 | Calcium Carbonate | HCID 10112 | — |
| 反応物 | 7-Amino-2,4-dichloro-6-fluorobenzothiazole | HCID 19933457 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,4-Dichloro-6-fluoro-7-isothiocyanatobenzothiazole | HCID 19933464 | — |
反応手順
A suspension of 16.9 g calcium carbonate in 100 ml water was added to a solution of 19.4 g thiophosgene in 100 ml dichloromethane. A solution of 40 g 7-amino-2,4-dichloro-6-fluorobenzothiazole in 500 ml dichloromethane was added, dropwise at 5° C., and the mixture stirred for 8 hours at room temperature. The solid was filtered, the phases were separated, and the organic phase dried over magnesium sulfate and concentrated. The residue was purified by column chromatography (eluent: hexane/ethyl acetate). Yield: 16 g=38% of theory m.p.: 80°-81° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05424443 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-4a8947eb6a0041508dc83e1f4689d2d3 |
| 出典メモ | uspto-grants-1995_06 |