참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 1-(Trimethylsilyl)methylamine | HCID 87488 | — |
| 반응물 | 4-Bromo-3-chlorobenzoic acid | HCID 12594302 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-bromo-3-chloro-N-trimethylsilanylmethyl-benzamide | HCID 66836699 | 100% |
반응 단계
To a suspension of 4-bromo-3-chlorobenzoic acid (25.00 g, 106.2 mmol) in CH2Cl2 (320 mL) was added N,N-dimethyl aminopyridine (1.95 g), followed by N-ethyl-N-dimethylamine propylcarbodiimide hydrochloride (22.39 g) in small portions. After 30 min at room temperature, aminomethyl trimethylsilane (11.2 g, 7.87 mL, 108 mmol) was added while maintaining the temperature at 20° C. After stirring over night, water was added and the organic layer was separated. The aqueous layer was extracted twice with CH2Cl2 and the combined organic phases were dried and evaporated in vacuum. The residue was purified by flash chromatography on silica gel to give the title compound (34.00 g, 100%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08653000B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_02 |
|---|
| ORD ID | ord-e86fb4dcd46743ff948c85722bfc7573 |
|---|
| 출처 메모 | uspto-grants-2014_02 |
|---|