関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Amino-4-chlorobenzenethiol | HCID 12000 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | Propanoyl chloride, 3-bromo- | HCID 84944 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-((2-Amino-4-chlorophenyl)thio)-1-(pyrrolidin-1-yl)propan-1-one | HCID 86690995 | 50.9% |
反応手順
To a solution of K2CO3 (3.6 g, 26 mmol) in THF (20 ml) was added pyrrolidine (2.1 ml, 26 mmol) at room temperature, then the mixture was cooled to −78° C. and 3-bromopropanoyl chloride (1.0 g, 5.83 mmol) was added slowly. After it was stirred for 30 min, 2-amino-4-chlorobenzenethiol (837 mg, 5.24 mmol) was added to the mixture and the reaction was stirred at room temperature for 3 hours. The mixture was diluted with water, extracted with EtOAc. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (0˜30% EtOAc in hexane) to yield the title compound (760 mg, 46%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822530B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-407ee69d0d2446c7b08cd2559c4e95aa |
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| 出典メモ | uspto-grants-2014_09 |
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