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Hydrochloric Acid → 4-Dimethylthiocarbamoyloxy-7-phenoxy-isoquinoline-3-carboxylic acid butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dabco | HCID 9237 | — |
| 反応物 | Dimethylthiocarbamoyl chloride | HCID 27871 | — |
| 反応物 | 4-Hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid butyl ester | HCID 66712951 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Dimethylthiocarbamoyloxy-7-phenoxy-isoquinoline-3-carboxylic acid butyl ester | HCID 86595464 | — |
反応手順
To a solution of 1.5 g of 4-Hydroxy-7-phenoxy-isoquinoline-3-carboxylic acid butyl ester, Example A-65.f, in 6.3 ml of anhydrous DMF was added 578 mg of dimethylthiocarbamoylchloride and 1.5 g of 1,4-diazabicyclo[2.2.2]octane. The mixture was stirred overnight at room temperature. The mixture was poured into 30 ml of 1 N HCl and extracted three times with 30 ml portions of ethyl acetate. The organic fractions were washed with water and brine, dried over anhydrous sodium sulfate, and concentrated to 1.9 g of product; MS (+) m/z 425.27 (M+1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863292B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-07e455f0c08a411a83b95c0267b16cb4 |
| 出典メモ | uspto-grants-2011_01 |