関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Trifluoroacetic anhydride | HCID 9845 | — |
| 反応物 | Piperazine, hydrochloride (1:?) | HCID 82044 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ammonium Hydroxide | HCID 14923 | 28% |
| 生成物 | 4-Trifluoroacetyl-2-(r,s)-(1-pyrrolidinyl)methyl piperazine | HCID 22707126 | — |
反応手順
To a solution of (R,S)2-(1-pyrrolidinyl)methyl]piperazine hydrochloride (1.0 g, 3.58 mmol) and Et3N (0.5 mL, 3.58 mmol) in 10 mL of CH2Cl2 was added trifluoroacetic anhydride (0.5 mL, 3.58 mmol) at 0° C. The reaction mixture is stirred at 0° C. for 5 h. The reaction mixture was evaporated under reduced pressure (due to the water solubility of this compound there was no aqueous work-up) and isolated on a silica gel column (solvent system: CH2Cl2: CH3OH: 28% NH4OH (98:2:2) to give the desired product as a free base (0.18 g, 20%); 1H NMR (free base 200 MHz, CDCl3) d 1.76 (m,4H), 2.25-3.15 (m, 10H), 3.26 (t, 2H), 3.88 (m, 1H), 4.39 (t, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06750216B2 |
|---|
| 出典データセット | uspto-grants-2004_06 |
|---|
| ORD ID | ord-afbdb6e0852c4d6b9a5d57ce6b0a2957 |
|---|
| 出典メモ | uspto-grants-2004_06 |
|---|
