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Water → 4-Chloro-4'-methylsulfonylmethylbenzophenone-semicarbazone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Chlorosulfonyl isocyanate | HCID 70918 | — |
| 反応物 | 4-Chloro-4'-methylsulfonylmethylbenzophenone-hydrazone | HCID 86752279 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 4-Chloro-4'-methylsulfonylmethylbenzophenone-semicarbazone | HCID 54202325 | 81.5% |
反応手順
4-chloro-4'-methylsulfonylmethylbenzophenone-hydrazone (1.3 g) and chlorosulfonyl isocyanate (0.63 g) were added to ethyl acetate (100 ml), and the mixture was stirred for one hour at room temperature. Then, water (100 ml) was added, and the mixture was further stirred for 16 hours at room temperature. The reaction mixture was subjected to liquid separation, and the ethyl acetate layer was washed with water and then dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure. The residual solid was washed with a solvent mixture of ethyl acetate:n-hexane=4:1, to obtain the desired product (1.2 g, melting point: 189° to 191° C., yield: 80%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05728699 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-71fa5a93fb9c483491defb7a5b1de773 |
| 出典メモ | uspto-grants-1998_03 |