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Dimethylformamide → 3-(4-chlorobenzylidene)-1H-naphtho[2,1-b][1,4]thiazin-2(3H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 4-Chlorobenzaldehyde | HCID 7726 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 1H-Naphtho[2,1-b][1,4]thiazin-2(3H)-one | HCID 13823452 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(4-chlorobenzylidene)-1H-naphtho[2,1-b][1,4]thiazin-2(3H)-one | HCID 53764522 | 52.8% |
反応手順
A mixture of 1H-naphtho[2,1-b][1,4]thiazin-2(3H)-one (5.17 g), 4-chlorobenzaldehyde (5.62 g), sodium methoxide (1.73 g) and dimethylformamide (80 ml) is refluxed for 4.5 hours. After cooling, the reaction mixture is poured into water and the resulting precipitate is separated by filtration, washed and dried and then is recrystallized from tetrahydrofuran-n-hexane to give 3-(4-chlorobenzylidene)-1H-naphtho[2,1-b][1,4]thiazin-2(3H)-one (4.28 g). M.p. 277°-279° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246929 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-f9dddaae649d44ff923cca915bde63f6 |
| 出典メモ | uspto-grants-1993_09 |