関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Methyl-alpha,alpha-diphenyl-4-piperidinemethanol | HCID 201485 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Piperidine, 4-(diphenylmethylene)-1-methyl- | HCID 95734 | 71.1% |
反応手順
Compound 9 (2.0 g, 6.41 mmol., 1.0 eq.), K2CO3 (1.77 g, 12.82 mmol., 2.0 eq.), halide (5.28 g, 32.05 mmol., 5.0 eq.) and DMF (25.0 mL) were combined and heated to 100° C. overnight. The crude reaction mixture was mixed with H2O (30 mL) and CH2Cl2 (35 mL). The organic phase was separated and the aqueous phase was washed with CH2Cl2 (2×25 mL). The combined organic phase was washed with brine and concentrated. The crude material was purified on a silica column to give compound 10 (1.2 g). The structure was confirmed by 1H NMR and LC/MS.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07355042B2 |
|---|
| 出典データセット | uspto-grants-2008_04 |
|---|
| ORD ID | ord-0faf32c6e20c4a04aeed8c18448b5ed8 |
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| 出典メモ | uspto-grants-2008_04 |
|---|
