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N-(4-Ethoxy-5-methylcarbamoylpyridin-2-ylmethyl)-N'-(fluoren-9-ylmethyloxycarbonyl)thiourea → 9H-Fluoren-9-ylmethyl (7-ethoxy-6-methylcarbamoyl-2H-imidazo[1,5-a]pyridin-3-ylidene)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-(4-Ethoxy-5-methylcarbamoylpyridin-2-ylmethyl)-N'-(fluoren-9-ylmethyloxycarbonyl)thiourea | HCID 57791308 | — |
| 触媒 | Mercury bis(trifluoroacetate) | HCID 2723924 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 9H-Fluoren-9-ylmethyl (7-ethoxy-6-methylcarbamoyl-2H-imidazo[1,5-a]pyridin-3-ylidene)carbamate | HCID 178465836 | — |
反応手順
875 mg of N-(4-ethoxy-5-methylcarbamoyl pyridin-2-ylmethyl)-N′-(fluoren-9-ylmethyloxycarbonyl)thiourea (Example 19a, crude product) were dissolved in 25 ml of dioxane and treated at RT with 837 mg (1.96 mmol) of mercury(II) trifluoroacetate. After 10 minutes, the mixture was concentrated and the residue was taken up in DCM. The organic phase was washed three times with 4% strength LiCl solution and once with water, dried with MgSO4 and concentrated in a rotary evaporator. The crude product thus obtained (590 mg) was reacted further without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863269B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-8b381985904d458e8891b45a0d720ba1 |
| 出典メモ | uspto-grants-2011_01 |