Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylamine, hydrochloride → 2-chloro-N,N-dimethyl-4-nitrobenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 반응물 | Benzoyl chloride, 2-chloro-4-nitro- | HCID 81522 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-chloro-N,N-dimethyl-4-nitrobenzamide | HCID 3264553 | — |
반응 단계
2-chloro-4-nitrobenzoyl chloride Compound 13a1 (7.08 g, 32.2 mmol) and dimethylamine hydrochloride (2.62 g, 32.2 mmol) were combined in THF (50 mL) at 0° C. TEA (8.97 mL, 64.4 mmol) was added and the mixture was heated at reflux for 18 hrs. When the reaction was complete, the mixture was diluted with 1N HCl and extracted with EtOAc. The product was isolated by flash chromatography (30-50% EtOAc/hexane gradient) to provide 2-chloro-N,N-dimethyl-4-nitro-benzamide Compound 13a2 (3.05 g) as a tan solid. MS 229 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07659284B2 |
| 출처 데이터셋 | uspto-grants-2010_02 |
| ORD ID | ord-6fd098a910c04dc3a2df9164f9949f82 |
| 출처 메모 | uspto-grants-2010_02 |