関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | 2-(2-Methoxyphenyl)acetyl chloride | HCID 179502 | — |
| 反応物 | HCID 178464632 | HCID 178464632 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | HCID 178464623 | HCID 178464623 | — |
反応手順
8.80 g of a 50% aqueous sodium hydroxide solution, ethylguanidine sulfate (14.98 g) and 100 ml of acetone, are stirred for 21/2 hrs at RT. The resulting mixture is treated with anhydrous sodium sulfate (6.0 g) and stirring continued for 1 hr. A solution of 2-methoxyphenylacetyl chloride (9.23 g) in 50 ml of acetone is added to the mixture dropwise and stirring is continued overnight at RT. The reaction mixture is filtered, the filtrate diluted with 100 ml of saturated aqueous sodium bicarbonate and the acetone evaporated in vacuo. The residue is diluted with 100 ml H2O and extracted with two 100 ml portions of methylene chloride. The extract is dried with sodium sulfate, filtered and concentrated in vacuo. The concentrate is acidified with ethereal hydrochloric acid and the solvent evaporated in vacuo. After stirring the residue with 200 ml of diethyl ether, the solid is collected, washed with diethyl ether and dried in air. The residual solid is recrystallized from acetone affording a white solid, M.P. 127°-128° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04544670 |
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| 出典データセット | uspto-grants-1985_10 |
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| ORD ID | ord-b6b66047a33245c88c41721924bdcb07 |
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| 出典メモ | uspto-grants-1985_10 |
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