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Trifluoroacetic acid → (+/-)-5-[7-Ethyl-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl]-1-methyl-2,4(1H,3H)-pyrimidinedione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 1-Methyluracil | HCID 12009 | — |
| 反応物 | (+/-)-7-Ethyl-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-ol | HCID 70113719 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (+/-)-5-[7-Ethyl-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl]-1-methyl-2,4(1H,3H)-pyrimidinedione | HCID 70113042 | — |
反応手順
1-Methyluracil (0.064 g) was added to a solution of the product from step (xi) (0.10 g) in dichloromethane (2 ml), followed by trifluoroacetic acid (1 ml). The orange solution was stirred at room temperature for 10 minutes before the solvent was removed under reduced pressure. The residue was azeotroped twice with acetonitrile, and the crude product purified by chromatography, eluting with 0-5% methanol in ethyl acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06218376B1 |
| 出典データセット | uspto-grants-2001_04 |
| ORD ID | ord-f8231aed488949d49c4339c3952f52d4 |
| 出典メモ | uspto-grants-2001_04 |