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Methylamine → methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 2-Thiophenecarboxylic acid, 3-(chlorosulfonyl)-, methyl ester | HCID 2736733 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate | HCID 12906749 | — |
反応手順
To a solution of methyl 3-(chlorosulfonyl)thiophene-2-carboxylate (500 mg, 2.077 mmol) in DCM (20 ml), methanamine 2N solution in THF (4.155 ml, 8.31 mmol) was added and the reaction was stirred for 1 hour at RT. The mixture was partitioned between 2N HCl and DCM and the aqueous phase was extracted with DCM. The combined organic layers were dried over sodium sulfate and the solvent was removed affording methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate (Int. 32) (430 mg, 1.828 mmol, MS/ESI+235.8 [MH]+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440954B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-9b66d920a79c456da03aea4e17f10758 |
| 出典メモ | uspto-grants-2016_09 |