참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | (Diethylamino)sulfur trifluoride | HCID 123472 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 1,1-Dimethylethyl 3-cyano-3-(hydroxymethyl)-1-azetidinecarboxylate | HCID 58438953 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Tert-butyl 3-cyano-3-(fluoromethyl)azetidine-1-carboxylate | HCID 58293513 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08193378B2 |
|---|
| 출처 데이터셋 | uspto-grants-2012_06 |
|---|
| ORD ID | ord-3a948117613649c2a92702f858a50e0a |
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| 출처 메모 | uspto-grants-2012_06 |
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