Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 375679생성일: 2026년 10월 23일
Sodium hydride → N,N-dimethyl-2-chloro-5-[3,6-dihydro-4-trifluoromethyl-2,6-dioxo-1(2H)-pyrimidinyl]-benzenesulfonamide
https://huagongshe.com/ko/reaction/375679
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ethyl 3-amino-4,4,4-trifluoro-2-butenoate | HCID 136209 | — |
| 반응물 | N,N-dimethyl-2-chloro-5-isocyanatobenzenesulfonamide | HCID 18993674 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | N,N-dimethyl-2-chloro-5-[3,6-dihydro-4-trifluoromethyl-2,6-dioxo-1(2H)-pyrimidinyl]-benzenesulfonamide | HCID 18993677 | — |
반응 단계
To 30 ml of dried tetrahydrofuran (THF) cooled to -5° C. was added, under nitrogen, 3.6 g of sodium hydride as a 60% dispersion mineral oil. To the stirred slurry was added a solution of 10 g of ethyl 3-amino-4,4,4-trifluoro-2-butenoate in 30 ml of THF over a period of 30 minutes. After stirring at -5° C. for 1 hour, the reaction mixture was cooled to -65° C. and a solution of N, N-dimethyl-2-chloro-5-isocyanatobenzenesulfonamide (Example A-4 above) in 30 ml of THF was added dropwise maintaining the temperature below -60° C. The mixture was stirred at -65° C. for 2 hours and allowed to warm to room temperature. After stirring for 17 hours, solvent was removed using a rotary evaporator. About 50 ml of water was added to the residue. The resulting mixture was filtered to remove a small amount of undissolved solid and the filtrate was acidified with hydrochloric acid. The resulting precipitate was filtered to give 13 g of the title compound as a beige solid, m.p. 281°-283° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05486610 |
|---|
| 출처 데이터셋 | uspto-grants-1996_01 |
|---|
| ORD ID | ord-cfa816a3e3654cc0a5c76a5f9d7681d5 |
|---|
| 출처 메모 | uspto-grants-1996_01 |
|---|