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Potassium Carbonate → 2-Chloro-5-(3-diethylamino-1-propoxy)nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-(Diethylamino)-1-propanol | HCID 12159 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 4-Chloro-3-nitrophenol | HCID 69127 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloro-5-(3-diethylamino-1-propoxy)nitrobenzene | HCID 22014731 | 90.7% |
反応手順
MsCl (6.0 mmol) was added dropwise at 0° C. to a stirred solution of 3-diethylamino-1-propanol (6.0 mmol), TEA (6.0 mmol) in anhydrous DCM (6 mL), and the mixture was stirred at the same temperature for 10 min, and at room temperature for additional 1 h. After the removal of the solvent in vacuo, the solid residue was mixed with 4-chloro-3-nitrophenol (5.0 mmol), and K2CO3 (10 mmol) in anhydrous DMF (10 mL), following the general procedure III (Step A). The crude product is purified using silica gel column chromatography 5% MeOH/DCM as eluent to yield 2-chloro-5-(3-diethylamino-1-propoxy)nitrobenzene (1.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087632B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-a2ee85c640ce4339a5e720ec558b5af4 |
| 出典メモ | uspto-grants-2006_08 |