関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Nitrobenzyl bromide | HCID 66011 | — |
| 反応物 | 5-(4-Chlorophenyl)-3,6-dihydro-1,3,4-thiadiazin-2-one | HCID 329473 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 66636793 | HCID 66636793 | — |
反応手順
To a solution of the compound obtained in Step A (57.83 mmoles) in acetonitrile (260 ml) there are added 1-bromomethyl-4-nitro-benzene (63.61 mmoles) and potassium carbonate (231.32 mmoles). The reaction mixture is stirred at 80° C. for 1 hour under nitrogen. The reaction mixture is brought to ambient temperature and 100 ml of water are added. Extraction with ethyl ether (3×350 ml) is carried out and the organic phases are combined. The organic phase obtained is dried over sodium sulphate, filtered and evaporated to dryness. The solid is triturated in ethyl ether, filtered off and dried in vacuo to yield the title product, which is used directly in the next Step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08541412B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-02652757b88b4162a185048b91d42468 |
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| 出典メモ | uspto-grants-2013_09 |
|---|
