関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | Ethyl 2-amino-4-chlorothieno(2,3-d)pyrimidine-6-carboxylate | HCID 16096301 | — |
| 触媒 | Zinc cyanide (Zn(CN)2) | HCID 11186 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 触媒 | Ferrocene-1,1'-bis-(diphenylphosphine) | HCID 635956 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 生成物 | 2-Amino-4-cyano-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester | HCID 59519342 | — |
反応手順
2-Amino-4-chloro-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl ester (1 equiv.), Zn(CN)2 (0.6 equiv.), Zn dust (0.12 equiv.), Pd2(dba)3 (0.02 mole eq.) and 1,1′-bis(diphenylphosphino)ferrocene (0.04 equiv.) were mixed in DMA and the mixture was stirred under argon at 120° C. for 24 hours. The resulting suspension was filtered through a short Celite column, the filtrate was diluted with brine and extracted with ethyl acetate. The organic layer was then washed with brine, water and dried over sodium sulphate. After evaporation of the solvent, the crude oil was purified by preparative TLC.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07820658B2 |
|---|
| 出典データセット | uspto-grants-2010_10 |
|---|
| ORD ID | ord-03a2198650744cf0b03645c84c4583b0 |
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| 出典メモ | uspto-grants-2010_10 |
|---|
