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Triethylamine → tert-Butyl 2-[4-(3,4-dichlorophenoxy)-1-piperidinyl]ethylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-(3,4-Dichlorophenoxy)piperidine | HCID 3732042 | — |
| 反応物 | tert-Butyl N-(2-bromoethyl)carbamate | HCID 4103526 | — |
| 反応物 | Diethylether water | HCID 21584184 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | tert-Butyl 2-[4-(3,4-dichlorophenoxy)-1-piperidinyl]ethylcarbamate | HCID 22322299 | 73.8% |
反応手順
The product from Example 1 Step (b) (8.6 g) was dissolved in DMF (60 ml) and triethylamine (12 ml) was added. tert-Butyl 2-bromoethylcarbamate (7.8 g) was added and the solution stirred at room temperature for 12 hours. Diethyl ether/H2O (1:1 500 ml) added and the organic phase separated, dried with MgSO4 and evaporated to a gum. Purification by flash chromatography (dichloromethane: methanol: 880 NH3 (aq) 98.5:1:0.5) gave the sub-title product (10 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07304077B2 |
| 出典データセット | uspto-grants-2007_12 |
| ORD ID | ord-b6cbc81e04614e9785818f367e3a0680 |
| 出典メモ | uspto-grants-2007_12 |