Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dichloroethane → HCID 178451952, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | 1,2,3-Thiadiazol-5-amine | HCID 77736 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 1,2-Pyrrolidinedicarboxylic acid, 1-(1,1-dimethylethyl) ester, (2S)- | HCID 85083 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 178451952 | HCID 178451952 | — |
반응 단계
Boc-L-Proline (9.7 g, 45.2 mmol), 4-phenyl-1,2,3,-thiadiazol-5-amine (4.0 g, 22.6 mmol), EDC (8.2 g, 42.9 mmol), HOBt (5.8 g, 42.9 mmol), DIPEA (19.7 ml, 113 mmol) were combined and stirred for 3 days in 40 ml DMF at 60 deg C. Ethyl acetate and saturated aqueous NaHCO3 were added. The aqueous layer was separated and extracted with ethyl acetate. Organic layers were combined and washed with aqueous NaHCO3 and brine. Organic layer was dried over MgSO4 and concentrated to a brown residue. Pure Boc-prolyl-4-phenyl-5-amino-1,2,3-thiadiazole c was obtained by crystallization from 100 ml hot acetonitrile to obtain 5.9 g. Calculated mass 374.5. found 375.3.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08907092B2 |
| 출처 데이터셋 | uspto-grants-2014_12 |
| ORD ID | ord-92430ae85e3449c381d63675680a8fa8 |
| 출처 메모 | uspto-grants-2014_12 |