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Potassium Carbonate → HCID 68793197、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,3-Dioxolane-2-ethylamine | HCID 79827 | — |
| 反応物 | 3-fluoro-N,N-bis(3-methylbutyl)-4-nitrobenzamide | HCID 68447111 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 68793197 | HCID 68793197 | 98% |
反応手順
A mixture of 3-fluoro-N,N-bis(3-methylbutyl)-4-nitrobenzamide prepared according to Example A1 (1.86 g, 1 eq), 2-(2-aminoethyl)-1,3-dioxolane (0.8 g, 1.2 eq) and potassium carbonate (1.58 g, 2 eq) in acetonitrile (150 ml) is heated under reflux for 3 hours then concentrated under reduced pressure at 40° C. The residue is taken up in dichloromethane (150 ml) and water (60 ml). After decantation and extractions, the combined organic phases are washed with salt water, dried over Na2SO4 then concentrated under reduced pressure at 40° C. Purification of the residue by flash chromatography on silica gel (eluent: heptane/ethyl acetate 8:2 to 7:3) produces the expected compound in the form of an orange-yellow oil (2.4 g; 98% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07355052B2 |
| 出典データセット | uspto-grants-2008_04 |
| ORD ID | ord-8362d300df2b4fb980a2dfb34e5e6f6b |
| 出典メモ | uspto-grants-2008_04 |