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2,2-Difluoroethyl trifluoromethanesulfonate → tert-Butyl 2-[4-(5-chloro-2-cyanophenyl)-5-methoxy-2-oxopyridin-1(2H)-yl]-4,4-difluorobutanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,2-Difluoroethyl trifluoromethanesulfonate | HCID 2774089 | — |
| 反応物 | tert-Butyl [4-(5-chloro-2-cyanophenyl)-5-methoxy-2-oxopyridin-1(2H)-yl]acetate | HCID 117622654 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | tert-Butyl 2-[4-(5-chloro-2-cyanophenyl)-5-methoxy-2-oxopyridin-1(2H)-yl]-4,4-difluorobutanoate | HCID 117622830 | — |
反応手順
150 mg (388 μmol) of tert-butyl [4-(5-chloro-2-cyanophenyl)-5-methoxy-2-oxopyridin-1(2H)-yl]acetate, 125 mg (582 μmol) of 2,2-difluoroethyl trifluoromethanesulphonate and 427 μl (427 μmol) of bis(trimethylsilyl)lithium amide (1M in THF) in 3 ml of THF were reacted according to General Method 7B. Purification by column chromatography (24 g silica cartridge, flow rate: 35 ml/min, cyclohexane/ethyl acetate gradient) gave the title compound. Yield: 122 mg (71% of theory)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434690B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-b1454be2a85e43ecbdb6de7d2ecc27d9 |
| 出典メモ | uspto-grants-2016_09 |