Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Thiophosgene → 2,4-Dichloro-6-fluoro-7-isothiocyanatobenzothiazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Thiophosgene | HCID 10040 | — |
| 반응물 | Calcium Carbonate | HCID 10112 | — |
| 반응물 | 7-Amino-2,4-dichloro-6-fluorobenzothiazole | HCID 19933457 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2,4-Dichloro-6-fluoro-7-isothiocyanatobenzothiazole | HCID 19933464 | — |
반응 단계
A suspension of 16.9 g calcium carbonate in 100 ml water was added to a solution of 19.4 g thiophosgene in 100 ml dichloromethane. A solution of 40 g 7-amino-2,4-dichloro-6-fluorobenzothiazole in 500 ml dichloromethane was added, dropwise at 5° C., and the mixture stirred for 8 hours at room temperature. The solid was filtered, the phases were separated, and the organic phase dried over magnesium sulfate and concentrated. The residue was purified by column chromatography (eluent: hexane/ethyl acetate). Yield: 16 g=38% of theory m.p.: 80°-81° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05424443 |
| 출처 데이터셋 | uspto-grants-1995_06 |
| ORD ID | ord-4a8947eb6a0041508dc83e1f4689d2d3 |
| 출처 메모 | uspto-grants-1995_06 |