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Water → tert-Butyl 2-(3,4-dichlorophenylsulfonamido)-4,5,6,7-tetrahydrobenzo[b]-thiophene-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Benzenesulfonyl chloride, 3,4-dichloro- | HCID 7383 | — |
| 反応物 | tert-Butyl 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate | HCID 10777280 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | tert-Butyl 2-(3,4-dichlorophenylsulfonamido)-4,5,6,7-tetrahydrobenzo[b]-thiophene-3-carboxylate | HCID 86625455 | — |
反応手順
tert-Butyl 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate (12.26 g, 48.4 mmol) was dissolved in DCM (150 ml), and pyridine (6.0 ml, 74 mmol) was added thereto. A solution of 3,4-dichlorobenzenesulfonyl chloride (8.4 ml, 54 mmol) was then added, and the mixture was heated for 17 h under reflux and then cooled to room temperature. Water was added (100 ml), and stirring was carried out overnight at room temperature. The phases were then separated (pH organic phase≈2), washed with saturated NaHCO3 solution, dried (sodium sulfate) and concentrated in vacuo.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08119633B2 |
| 出典データセット | uspto-grants-2012_02 |
| ORD ID | ord-9b9e7296bb0049d68a884740daff09a0 |
| 出典メモ | uspto-grants-2012_02 |