참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1,6-Dibromohexane | HCID 12368 | — |
| 반응물 | 3-Hydroxybenzamide | HCID 342403 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-[(6-Bromohexyl)oxy]benzenecarboxamide | HCID 59402930 | 67% |
반응 단계
(Method D) K2CO3 (1.38 g, 10 mmol, 1 equiv.) was added to a suspension of 3-hydroxybenzamide (1.37 g, 10 mmol, 1 equiv.) in CH3CN (100 ml). The mixture stirred for 10 min at room temperature, before 1,6-dibromo-hexane (9.76 g, 40 mmol, 4 equiv.) was added. The resulting mixture was stirred at 60° C. for 16 h. After this time, the reaction was cooled to room temperature, any undissolved solids were filtered off and the filtrate evaporated under reduced pressure to dryness. The residue was taken-up in EtOAc and water. The organic phase was separated and washed consecutively with K2CO3 solution, water and brine. Dried with MgSO4 and evaporated under reduced pressure to a small volume. The precipitant solid was filtered and washed with EtOAc/pentane, to give the desired compound as a white solid (2.0 g, 67%), mp 115-117° C. HPLC-MS (method 1): m/z 300 [M]+, 302 [M+2H]+, Rt=4.08 min.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08088791B2 |
|---|
| 출처 데이터셋 | uspto-grants-2012_01 |
|---|
| ORD ID | ord-cab0fd9a957e427797afc213ab8967fb |
|---|
| 출처 메모 | uspto-grants-2012_01 |
|---|