関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | (Diethylamino)sulfur trifluoride | HCID 123472 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1,1-Dimethylethyl 3-cyano-3-(hydroxymethyl)-1-azetidinecarboxylate | HCID 58438953 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Tert-butyl 3-cyano-3-(fluoromethyl)azetidine-1-carboxylate | HCID 58293513 | — |
反応手順
tert-Butyl 3-cyano-3-(hydroxymethyl)azetidine-1-carboxylate (5.0 g) was dissolved in DCM (100 mL). At 0° C., DAST (3.74 mL) was added thereto, followed by stirring at 0° C. for 3 hours. Three hours later, to the reaction liquid was added an aqueous NaHCO3 solution (100 mL), followed by extraction with DCM (50 mL) three times. The organic layer was washed with brine, dried over MgSO4, and then concentrated. The residue was purified by silica gel column chromatography (automatic purification device, hexane:EtOAc=100:0 to 50:50) to obtain tert-butyl 3-cyano-3-(fluoromethyl)azetidine-1-carboxylate (1.24 g) as a brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08193378B2 |
|---|
| 出典データセット | uspto-grants-2012_06 |
|---|
| ORD ID | ord-3a948117613649c2a92702f858a50e0a |
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| 出典メモ | uspto-grants-2012_06 |
|---|
