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Oxalic Acid → N,N-Diethyl-N'-[2-(phenylsulfonyl)ethyl]-1,4-butanediamine oxalate hydrate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Oxalic Acid | HCID 971 | — |
| 反応物 | ((2-Chloroethyl)sulphonyl)benzene | HCID 13646 | — |
| 反応物 | N,N-Diethyl-1,4-butanediamine | HCID 117976 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N,N-Diethyl-N'-[2-(phenylsulfonyl)ethyl]-1,4-butanediamine oxalate hydrate | HCID 19869533 | 164.4% |
反応手順
A mixture of 28.2 g (0.138 mole) of [(2-chloroethyl)sulfonyl]benzene and 20.0 g (0.139 mole) of 4-(N,N-diethylamino)-1-butanamine in 700 ml of acetonitrile was stirred at room temperature for 16 hr. The solvent was removed in vacuo, and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over magnesium sulfate, and the solvent was removed in vacuo. The residue was dissolved in methanol, a solution of 25.0 g (0.278 mole) of oxalic acid was added and a precipitate was collected to give 47.69 g (68.9%) of title compound, a white crystalline solid, mp 158°-165° C. with decomposition.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04895840 |
| 出典データセット | uspto-grants-1990_01 |
| ORD ID | ord-c6dccbefbc6a4abbadf02e99b7bdf981 |
| 出典メモ | uspto-grants-1990_01 |