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Sodium Carbonate → 1-(2-Methoxy-5-trifluoromethoxybenzoyl)-3-phenyl-3-(2-hydroxyethyl)pyrrolidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Methoxy-5-(trifluoromethoxy)benzoyl chloride | HCID 3580596 | — |
| 反応物 | (-)-3-phenyl-3-(2-hydroxyethyl)pyrrolidine (R,R)-di-p-anisoyltartaric acid | HCID 70109704 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | 1-(2-Methoxy-5-trifluoromethoxybenzoyl)-3-phenyl-3-(2-hydroxyethyl)pyrrolidine | HCID 22009408 | — |
反応手順
Combine (−)-3-phenyl-3-(2-hydroxyethyl)pyrrolidine (R,R)-di-p-anisoyltartaric acid salt (1.7 g, 2.5 mmol) and sodium carbonate (1.32 g, 12.5 mmol) in ethyl acetate/water (1/1) (20 mL). Add a solution of 2-methoxy-5-trifluoromethoxybenzoyl chloride (0.64 g, 2.5 mmol) in ethyl acetate (10 mL). After 14 hours, separate the organic layer. Extract the aqueous layer four times with dichloromethane. Dry the combined organic layers over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with ethyl acetate to give the title compound: Rf=0.32 (silica gel, ethyl acetate).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06211199B1 |
| 出典データセット | uspto-grants-2001_04 |
| ORD ID | ord-401d2abe422342a5a74ab9324ab3f15a |
| 出典メモ | uspto-grants-2001_04 |