Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 2-Amino-4-(benzo[1,3]dioxol-5-yl-cyano-methyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 3,4-(Methylenedioxy)phenylacetonitrile | HCID 78178 | — |
| 반응물 | Ethyl 2-amino-4-chlorothieno(2,3-d)pyrimidine-6-carboxylate | HCID 16096301 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Sodium chloride; water | HCID 57417360 | — |
| 생성물 | 2-Amino-4-(benzo[1,3]dioxol-5-yl-cyano-methyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester | HCID 59519339 | — |
반응 단계
To a solution of 2-amino-4-chloro-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester (1 equiv.) and benzo[1,3]dioxol-5-yl-acetonitrile (1 mole eq.) in DMF at room temperature, sodium hydride (1.1 mole eq., 60% in mineral oil) was added. The mixture was stirred at this temperature overnight under argon. After that, it was diluted with brine and extracted with ethyl acetate. The combined organic portions were washed with brine and water and dried with sodium sulphate. After filtration and evaporation of the solvent, brown solids were obtained which were purified either by preparative TLC or preparative HPLC.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08642594B2 |
| 출처 데이터셋 | uspto-grants-2014_02 |
| ORD ID | ord-531272634c83410985e09d780a325f76 |
| 출처 메모 | uspto-grants-2014_02 |