Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 5-Methylthio-6-trifluoromethyl-1-[3-[(2-dimethylaminoethyl)carbamoyl]phenyl carbamoyl]indoline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | N,N-Dimethylethylenediamine | HCID 66053 | — |
| 반응물 | 5-Methylthio-6-trifluoromethyl-1-(3-carboxy Phenyl Carbamoyl)indoline | HCID 18005107 | — |
| 촉매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-Methylthio-6-trifluoromethyl-1-[3-[(2-dimethylaminoethyl)carbamoyl]phenyl carbamoyl]indoline | HCID 9956174 | 45% |
반응 단계
To a suspension of 5-methylthio-6-trifluoromethyl-1-(3-carboxy phenyl carbamoyl) indoline (0.5 g, 1.26mmol) in dichloromethane (20 ml) was added oxalyl chloride (0.3 ml, 2.52 mmol) and dimethylformamide (3 drops). After effervescing had subsided the reaction mixture was evaporated to dryness under reduced pressure. It was then dissolved in tetrahydrofuran (30 ml) and added to a solution of N,N-dimethylethylenediamine (0.405 g, 6.33mmol) and triethylamine (0.2 ml, 1.4 mmol) in tetrahydrofuran at 0° C. After 2 hours the reaction mixture was basified with 5M NaOH and water was added forming a white precipitate. This was filtered and dried to give the product a white solid (0.25 g, 45%), m.p. 91-93° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05972937 |
| 출처 데이터셋 | uspto-grants-1999_10 |
| ORD ID | ord-f8280e4dd96b47f9a1c79f68bf4aa884 |
| 출처 메모 | uspto-grants-1999_10 |