참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitrogen | HCID 947 | — |
| 반응물 | 2,6-Dimethoxynaphthalene | HCID 79627 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 반응물 | 4-(2-(Piperidin-1-yl)ethoxy)benzoyl chloride | HCID 11119066 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | (2,6-Dimethoxy-naphthalen-1-yl)-[4-(2-piperidin-1-yl-ethoxy)phenyl]-methanone | HCID 11654660 | 68% |
반응 단계
In a dry round bottom flask equipped with stir bar, temperature probe and N2 line, dissolve 2,6-dimethoxynaphthalene (1.0 eq) in CH2Cl2 (5 volume equivalents) at ambient temperature. Cool the solution to 0° C. in with an ice bath, and add 4-(2-piperidin-1-yl-ethoxy)-benzoyl chloride (1.1 eq). Add aluminum chloride (2.0 eq). Once the reaction is determined to be complete, quench the reaction slowly with 1 N NaOH and dilute with additional water and CH2Cl2. Wash the aqueous layer with (1×20 ML) of CH2Cl2. Combine the organic extracts and wash with brine and dry (Na2SO4). Recrystallize the crude product from methanol to give (2,6-dimethoxy-naphthalen-1-yl)-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-methanone (average yield 68%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07119206B2 |
|---|
| 출처 데이터셋 | uspto-grants-2006_10 |
|---|
| ORD ID | ord-0479db8dbca0419a9ea1f50068cdb019 |
|---|
| 출처 메모 | uspto-grants-2006_10 |
|---|