関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sarcosine | HCID 1088 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-Benzothiophene-3-sulfonyl chloride | HCID 2776340 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 22662727 | HCID 22662727 | — |
反応手順
6 g of NaOH, 23.27 g of 3-chlorosulphonyl-benzothiophene and 13.36 g of sarcosine are added to a mixture of 200 ml of toluene and 200 ml of water and stirred for 6.5 hours at 60° C. For working up, the aqueous phase is separated off and the organic phase is extracted with 100 ml of 2 N NaOH solution. The combined aqueous phases are acidified with conc. HCl and then extracted twice with 300 ml of ethyl acetate. After washing with saturated aqueous saline solution and drying over magnesium sulphate the organic phase is concentrated by evaporation. The crude product obtained is recrystallised from 100 ml of dichloroethane. Yield: 13.14 g. M.p.: 139-140° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06800623B2 |
|---|
| 出典データセット | uspto-grants-2004_10 |
|---|
| ORD ID | ord-03ec55e4e3684c609d2efaa8696f72b7 |
|---|
| 出典メモ | uspto-grants-2004_10 |
|---|
