Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → {2-[(2-Amino-benzothiazole-6-carbonyl)-amino]-phenyl}-carbamic acid tert-butyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 6-Benzothiazolecarboxylic acid, 2-amino- | HCID 66740 | — |
| 반응물 | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| 반응물 | N-(tert-Butoxycarbonyl)-1,2-phenylenediamine | HCID 676311 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | {2-[(2-Amino-benzothiazole-6-carbonyl)-amino]-phenyl}-carbamic acid tert-butyl ester | HCID 58930649 | 52% |
반응 단계
The acid 114 (1.80 g, 9.27 mmol) was combined with (2-amino-phenyl)-carbamic acid tert-butyl ester (2.31 g, 11.1 mmol) and BOP (4.91 g, 11.1 mmol) in DMF. To this solution Et3N (5.16 ml, 37.1 mmol) was added and the mixture was stirred overnight at room temperature under nitrogen, concentrated in vacuo and purified by flash column chromatography (30% hexane/EtOAc). To further purify the product, the mixture was partitioned between EtOAc and water, organic layer was separated, dried over MgSO4 and evaporated give the title compound 115 (1.84 g, 52%). 1H-NMR (DMSO) δ: 9.72 (s, 1H), 8.66 (m, 1H); 8.22 (d, J=1.8 Hz, 1H); 7.80 (m, 3H); 7.50 (m, 2H); 7.37 (m, 1H); 7.14 (m, 2H); 1.44 (s, 9H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08088805B2 |
| 출처 데이터셋 | uspto-grants-2012_01 |
| ORD ID | ord-43b2456e5de046fb85e66de78ee4d9a1 |
| 출처 메모 | uspto-grants-2012_01 |