Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chloroacetyl chloride → 1-(5-Acetyl-thiophen-2-yl)-2-chloro-ethanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chloroacetyl chloride | HCID 6577 | — |
| 반응물 | 2-Acetylthiophene | HCID 6920 | — |
| 반응물 | Chloromethyl Thienyl Ketone deriv. 5 | HCID 6539169 | — |
| 생성물 | 1-(5-Acetyl-thiophen-2-yl)-2-chloro-ethanone | HCID 4165708 | 25% |
반응 단계
General procedure described for compounds 1 and 2 starting from 2-acetylthiophene and chloroacetyl chloride. Purified by column chromatography column (hexane:ethyl acetate 3:1), yield 25%, m.p.: 94-95° C., 1H-NMR (CDCl3): δ8.3 (d, J=4.2 Hz, 1H, Ar), 8.1 (d, J=4.2 Hz, 1H, Ar), 4.55 (s, 2H, CH2), 2.6 (s, 3H, CH3); 13C-NMR (CDCl3). δ193.0 (CO), 187.8 (CO), 148.3 (C—CO), 142.0 (CH), 141.7 (C—CO), 133.7 (CH), 48.3 (CH2), 29.2 (CH3); M/z (EI): 204, 202 (M +, 4, 10%), 153 (M-CH2Cl, 100%); HPLC: Column μ Bondapack C18, 5 μm, 300 A, (300×3.9 mm), Purity 98%, r.t.=3.50 min, acetonitrile/H2O (0.05% H3PO4+0.04% Et3N) 50/50.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06747057B2 |
| 출처 데이터셋 | uspto-grants-2004_06 |
| ORD ID | ord-1ebba97bc0534d7e81d9088cc6554563 |
| 출처 메모 | uspto-grants-2004_06 |