Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chlorotrimethylsilane → 6-cyano-2-(2-(4-ethyl-3-(4-morpholinopiperidin-1-yl)phenyl)propan-2-yl)-1H-indole-3-carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chlorotrimethylsilane | HCID 6397 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Potassium Phosphate, Dibasic | HCID 24450 | — |
| 반응물 | Tert-butyl 6-cyano-2-(2-(4-ethyl-3-(4-morpholin-4-yl-piperidin-1-yl)phenyl)propan-2-yl)-1H-indole-3-carboxylic acid hydrochloric acid salt | HCID 66835223 | — |
| 용매 | Acetone | HCID 180 | — |
| 생성물 | 6-cyano-2-(2-(4-ethyl-3-(4-morpholinopiperidin-1-yl)phenyl)propan-2-yl)-1H-indole-3-carboxylic acid | HCID 66835218 | 96.6% |
반응 단계
Tert-butyl 6-cyano-2-(2-(4-ethyl-3-(4-morpholin-4-yl-piperidin-1-yl)phenyl)propan-2-yl)-1H-indole-3-carboxylic acid hydrochloric acid salt (1400 g) was suspended in TFE (7 L) under nitrogen stream, and added dropwise with TMSCl (554 ml) at 8° C. After stirring for 3 hrs, the reaction solution was added with acetone (5.6 L) and aqueous solution of NaOH (1 N, 4.39 L), and 10% aqueous solution of K2HPO4 (1.4 L) was added thereto for neutralization. The precipitated solid was filtered and collected, washed twice with a mixture solution of water:acetone (=1:1, 2.8 L), and dried to obtain the title compound (1061 g, 96.6%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09440922B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-4b4881646c254cb996144fcd8ef36721 |
| 출처 메모 | uspto-grants-2016_09 |