関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Tert-Butanesulfinamide | HCID 3382465 | — |
| 反応物 | 4-Chloro-2-fluoro-6-(3-methoxybenzoyl)benzonitrile | HCID 58579524 | — |
| 触媒 | Titanium tetraethoxide | HCID 76524 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-((5-chloro-2-cyano-3-fluorophenyl)(3-methoxyphenyl)methylene)-2-methylpropane-2-sulfinamide | HCID 76821604 | 59% |
反応手順
4-Chloro-2-fluoro-6-(3-methoxybenzoyl)benzonitrile (2.56 g, 8.84 mmol), 2-methyl-2-propanesulfinamide (1.392 g, 11.49 mmol) and titanium(IV) ethoxide (4.62 mL, 22.09 mmol) were dissolved in THF (30 mL) and stirred at 75° C. over weekend. When cooled to rt, the mixture was diluted with DCM (25 mL). Saturated aqueous NaHCO3 (3 mL) was added followed by silica and the mixture concentrated under reduced pressure until a free flowing powder was obtained. Purification on a silica gel column (0-40% EtOAc in heptane as eluent) gave 2.04 g (59% yield) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08030500B2 |
|---|
| 出典データセット | uspto-grants-2011_10 |
|---|
| ORD ID | ord-751b48230fcf4f98beb5a0f168bc0b32 |
|---|
| 出典メモ | uspto-grants-2011_10 |
|---|
