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Dicyclohexylcarbodiimide → HCID 15342494、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | N-(tert-butoxycarbonyl)glycine | HCID 78288 | — |
| 反応物 | Thieno[2,3-b]pyridin-3-amine | HCID 289923 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 15342494 | HCID 15342494 | 85.5% |
反応手順
1,3-Dicyclohexylcarbodiimide (11 g) was added with stirring to a solution of 3-aminothieno[2,3-b]pyridine (8 g) and N-(tert-butoxycarbonyl)glycine (10 g) in 200 mL of dichloromethane. After one hour the reaction mixture was filtered to remove the separated 1,3-dicyclohexylurea and evaporated to an oil. Crystallization from ethyl ether afforded 14 g of a solid, m.p. 190°-192° C. Recrystallization of 3 g from acetonitrile afforded 2.4 g of crystals, m.p. 192°-194° C. Final recrystallization from acetonitrile afforded 2.0 g of crystals, m.p. 194°-196° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05519032 |
| 出典データセット | uspto-grants-1996_05 |
| ORD ID | ord-ce41ca38361d40198b362580e4dbc8b1 |
| 出典メモ | uspto-grants-1996_05 |