関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4,6-Dichloro-5-(4-methylphenyl)pyrimidine | HCID 21979554 | — |
| 反応物 | 2-Phenyl-ethanesulfonic acid amide potassium salt | HCID 68898150 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Phenyl-ethanesulfonic acid (6-chloro-5-p-tolyl-pyrimidin-4-yl)-amide | HCID 86592469 | 59.6% |
反応手順
A solution of 2-phenyl-ethanesulfonic acid amide potassium salt (3.0 g), 4,6-dichloro-5-p-tolyl-pyrimidine (2.15 g) and Hunig's base (1.57 ml) in DMSO (50 ml) was stirred at rt for 20 h before it was diluted with water (500 ml) and extracted twice with diethyl ether (250 ml). The aqueous phase was acidified with acetic acid. The resulting suspension was cooled to 5° C. and filtered. The solid material was washed with water and diethyl ether, and dried at 40° C. under high vacuum to give 2-phenyl-ethanesulfonic acid (6-chloro-5-p-tolyl-pyrimidin-4-yl)-amide (2.08 g) as a grey powder. LC-MS: tR=5.23 min, [M+1]+=388.18, [M−1]−=386.14.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091201B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-de2c64610930487e978e7f18ba39fabb |
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| 出典メモ | uspto-grants-2006_08 |
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