Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → HCID 54137663, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | 1,2-Ethanediamine, N1,N1,N2-trimethyl- | HCID 67338 | — |
| 반응물 | 5-Methylthio-6-trifluoromethyl-1-(3-carboxy Phenyl Carbamoyl)indoline | HCID 18005107 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 54137663 | HCID 54137663 | 83.2% |
반응 단계
The carboxylic acid from Example 12 (0.5 g, 1.25 mmol) in dichloromethane (10 ml) was treated with oxalyl chloride (0.3 ml, 3.4 mol) and DMF (catalytic). Solution was stirred for 1 h and evaporated to dryness. The residue in dry THF (5 ml) was added to a stirred solution of triethylamine (0.3 ml, 4 mmol) and N,N,N'-trimethylethylenediamine (0.5 ml, 4.5 mmol) in dry THF (10 ml). Following 3 hours at room temperature, the solution was partitioned (H2O/EtOAc). Drying and removal of the organic layers followed by recrystallisation (EtOAc/60°-80° petrol) afforded the title compound (0.5 g, 83%) as a white solid. M.pt. 140°-141° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05972937 |
| 출처 데이터셋 | uspto-grants-1999_10 |
| ORD ID | ord-358a48d0a59041da99095b831ed2776a |
| 출처 메모 | uspto-grants-1999_10 |