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Benzoic acid, 2-chloro-5-(chlorosulfonyl)- → h-NTPDase8-IN-1
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoic acid, 2-chloro-5-(chlorosulfonyl)- | HCID 67306 | — |
| 反応物 | Cyclopropylamine | HCID 69828 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | h-NTPDase8-IN-1 | HCID 16768315 | 69.4% |
反応手順
To a solution of 2-chloro-5-(chlorosulfonyl)benzoic acid (4.0 g, 15.68 mmol) in DCM (60 mL) was added cyclopropyl amine (1.8 g, 31.57 mmol) and the reaction mixture was stirred at RT for 16 h. The reaction mass was concentrated and the residue was diluted with ice cold water and acidified with dilute HCl. The crude solid was filtered off, washed with water and dried to afford 3.0 g of pure product. 1H NMR (300 MHz, DMSO d6): δ 0.37 (s, 2H), 0.49 (d, J=5.4 Hz, 2H), 2.12-2.13 (m, 1H), 7.82 (d, J=8.4 Hz, 1H), 7.91 (d, J=8.4 Hz, 1H), 8.13 (s, 1H), 8.18 (s, 1H), 13.92 (br s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09439890B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-57f2ee6e028a4bac873e0a391adb8b2d |
| 出典メモ | uspto-grants-2016_09 |