Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chloroacetyl chloride → n-(5-Bromo-3-methyl-pyridin-2-yl)-2-chloro-acetamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chloroacetyl chloride | HCID 6577 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-Amino-5-bromo-3-methylpyridine | HCID 137934 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | n-(5-Bromo-3-methyl-pyridin-2-yl)-2-chloro-acetamide | HCID 52228026 | — |
반응 단계
1.75 mL (22 mmol) chloroacetyl chloride are added to a solution, cooled to 0° C., of 3.74 g (20 mmol) 2-amino-5-bromo-3-methylpyridine in 50 mL DCM and then 6.1 mL (44 mmol) triethylamine are slowly added dropwise. After the addition has ended the ice bath is removed and the reaction mixture is stirred for 4 h at RT. It is poured onto water, extracted exhaustively with DCM, the combined organic phases are washed with water and saturated NaCl solution and dried over Na2SO4. After the desiccant and solvent have been eliminated the residue is purified by chromatography (silica gel, cyc/EtOAc 2:1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08618132B2 |
| 출처 데이터셋 | uspto-grants-2013_12 |
| ORD ID | ord-4aede1005bfe4e03826578031574b8ca |
| 출처 메모 | uspto-grants-2013_12 |