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Ammonium Chloride → tert-butyl (+/-)-[(4aR*,8aS*)-8a-(6-amino-2,2-difluorobenzo[1,3]dioxol-4-yl)-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-2-yl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | tert-butyl (+/-)-[(4aR*,8aS*)-8a-(2,2-difluoro-6-nitrobenzo[1,3]dioxol-4-yl)-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-2-yl]carbamate | HCID 59281222 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | tert-butyl (+/-)-[(4aR*,8aS*)-8a-(6-amino-2,2-difluorobenzo[1,3]dioxol-4-yl)-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-2-yl]carbamate | HCID 59281180 | 89% |
反応手順
Iron powder (7.09 mg) and a saturated ammonium chloride solution (1.0 ml) were added to a solution of tert-butyl (±)-[(4aR*,8aS*)-8a-(2,2-difluoro-6-nitrobenzo[1,3]dioxol-4-yl)-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-2-yl]carbamate (60.0 mg) in ethanol (20 ml), and the mixture was heated under reflux for 30 minutes. The reaction solution was returned to room temperature and the insoluble matter was removed by filtration through celite. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography to obtain the title compound (50.0 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08198269B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-20c13fc941d848969a7f0d203b87fff9 |
| 出典メモ | uspto-grants-2012_06 |