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Water → tert-butyl (6SR,7SR)-7-(3,4-dichlorophenyl)-6-[(methylsulfonyl)amino]-1,4-oxazepane-4-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | tert-butyl (6SR,7SR)-6-amino-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate | HCID 66975299 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | tert-butyl (6SR,7SR)-7-(3,4-dichlorophenyl)-6-[(methylsulfonyl)amino]-1,4-oxazepane-4-carboxylate | HCID 66976033 | 82.2% |
反応手順
Methanesulfonyl chloride (34 mg) was added to a solution of tert-butyl (6SR,7SR)-6-amino-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (90 mg) and triethylamine (33 mg) in THF (5 mL), and the mixture was stirred at room temperature for 1 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (90 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08722662B2 |
| 出典データセット | uspto-grants-2014_05 |
| ORD ID | ord-870da08f2e68436e8367b1e693122630 |
| 出典メモ | uspto-grants-2014_05 |