化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 4-(9-cyclopentyl-5-ethyl-7,7-difluoro-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2486-69-3 | HCID 288057 | — |
| 反応物 | 2-Chloro-9-cyclopentyl-5-ethyl-7,7-difluoro-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one | HCID 86637505 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(9-cyclopentyl-5-ethyl-7,7-difluoro-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-benzoic acid | HCID 58015161 | 66.7% |
反応手順
A mixture of 0.30 g (0.91 mmole) 2-chloro-9-cyclopentyl-5-ethyl-7,7-difluoro-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VII-138) and 0.18 g (1.09 mmole) 4-amino-3-methoxy-benzoic acid in a 1:4 mixture of 5 mL of ethanol and 1 M hydrochloric acid was heated at 100 degrees for 18 hours. After cooling, the precipitate was collected by filtration, washed with water and dried to give 0.28 g of 4-(9-cyclopentyl-5-ethyl-7,7-difluoro-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-benzoic acid (I-156).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08003785B2 |
| 出典データセット | uspto-grants-2011_08 |
| ORD ID | ord-5bff33837d3d43cb9db35efa1f4f9fe9 |
| 出典メモ | uspto-grants-2011_08 |