Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Toluene → 5-tert.Butylcarbamylphthalid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Tert-Butylamine | HCID 6385 | — |
| 반응물 | 1,3-Dihydro-1-oxoisobenzofuran-5-carboxylic acid | HCID 78517 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Thionyl Chloride | HCID 24386 | — |
| 생성물 | 5-tert.Butylcarbamylphthalid | HCID 11148992 | — |
반응 단계
5-Carboxyphthalid (36 g, 0.2 mole) is suspended in thionylchloride (100 mL). DMF (1.5 mL) is added and the mixture is refluxed for 1 hour. Toluene (200 mL) is added and the solvents are evaporated in vacuo. The residue is dissolved in THF (200 mL) and added to a solution of tert.butylamine (31 g, 0.42 mole) in THF (200 mL) at 5° C. The mixture is allowed to warm to room temperature and stirred overnight. The reaction is then poured into ice water (400 mL) and the precipitated crystals are filtered off. The crystals are washed with water (100 mL). Yield: 41 g, 87%. DSC onset: 189.5° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06229026B1 |
| 출처 데이터셋 | uspto-grants-2001_05 |
| ORD ID | ord-94938be2fcd0455e9ea8ccdb7d16aa64 |
| 출처 메모 | uspto-grants-2001_05 |