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1,1-bis(1,1-dimethylethoxy)-N,N,N-trimethylamine → 6-[(Dimethylamino)methylene]-4,5,6,7-tetrahydro-1,4,4-trimethyl-7-oxo-1H-indazole-3-carboxylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1-bis(1,1-dimethylethoxy)-N,N,N-trimethylamine | HCID 547712 | — |
| 反応物 | Ethyl 1,4,4-trimethyl-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate | HCID 44235648 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-[(Dimethylamino)methylene]-4,5,6,7-tetrahydro-1,4,4-trimethyl-7-oxo-1H-indazole-3-carboxylic acid ethyl ester | HCID 68934344 | 87.1% |
反応手順
A solution of ethyl 1,4,4-trimethyl-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate (4.8 g, 19.18 mmol) in anhydrous dimethylformamide (30 mL) was treated with dimethylformamide di-tert-butylacetal (9.19 mL, 38.35 mmol) at 65° C. for 2 hours. The mixture was evaporated to dryness and the crude material was crystallized from hexane to give the title compound (5.1 g, 87% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541429B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-f8901392c59347cf94cea587180b5417 |
| 出典メモ | uspto-grants-2013_09 |