Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → 2-Chloro-5-(3-diethylamino-1-propoxy)nitrobenzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3-(Diethylamino)-1-propanol | HCID 12159 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | 4-Chloro-3-nitrophenol | HCID 69127 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-Chloro-5-(3-diethylamino-1-propoxy)nitrobenzene | HCID 22014731 | 90.7% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07087632B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-a2ee85c640ce4339a5e720ec558b5af4 |
| 출처 메모 | uspto-grants-2006_08 |