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Water → Methyl [4-cyano-1-(trifluoroacetyl)-2,3-dihydro-1h-1-benzazepin-2-yl]acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,4,7,10-Tetraoxacyclododecane | HCID 9269 | — |
| 反応物 | Methyl (1-(trifluoroacetyl)-4-{[(trifluoromethyl)sulphonyl]oxy}-2,3-dihydro-1h-1-benzazepin-2-yl)acetate | HCID 91577583 | — |
| 反応物 | HCID 178506913 | HCID 178506913 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Methyl [4-cyano-1-(trifluoroacetyl)-2,3-dihydro-1h-1-benzazepin-2-yl]acetate | HCID 91539061 | — |
反応手順
A solution of the compound obtained in Step e (1.35 g; 293 mmol) in 16 ml of anhydrous toluene is added to a mixture of LiCN (0.5 M in DMF) (11.72 ml; 5.86 mmol), (Ph3P)4Pd (237 mg; 0.205 mmol) and 12-crown-4 (36 mg; 0.205 mmol) under an argon. atmosphere. The reaction mixture is stirred at ambient temperature for 6 hours. Water (10 ml) is added to the reaction mixture, and the organic phase is extracted with diethyl ether. After drying and concentration, the residue obtained is purified on silica gel (eluant:heptane/EtOAc) to yield the title product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06846833B2 |
| 出典データセット | uspto-grants-2005_01 |
| ORD ID | ord-509b45decb944185882a990907552a84 |
| 出典メモ | uspto-grants-2005_01 |