反応式
[CH3:1][C@H:2]1[NH:7][C@@H:6]([CH3:8])[CH2:5][N:4]([C:9]2[CH:10]=[CH:11][C:12]([O:16][CH3:17])=[C:13]([CH:15]=2)[NH2:14])[CH2:3]1.CN1CCOCC1.[Br:25][C:26]1[C:31]([F:32])=[CH:30][C:29]([S:33](Cl)(=[O:35])=[O:34])=[C:28]([F:37])[CH:27]=1>ClCCl>[Br:25][C:26]1[C:31]([F:32])=[CH:30][C:29]([S:33]([NH:14][C:13]2[CH:15]=[C:9]([N:4]3[CH2:3][C@H:2]([CH3:1])[NH:7][C@H:6]([CH3:8])[CH2:5]3)[CH:10]=[CH:11][C:12]=2[O:16][CH3:17])(=[O:34])=[O:35])=[C:28]([F:37])[CH:27]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
A solution of 5-(cis-3,5-dimethyl-1-piperazinyl)-2-(methyloxy)aniline (D4) (500 mg, 2.12 mmol) in dichloromethane (30 ml) was treated with morpholinomethyl-polystyrene HL resin (1 g, 4 mmol/g loading, 4.24 mmol) followed by 4-bromo-2,5-difluorobenzene sulfonyl chloride (930 mg, 3.2 mmol). The resulting solution was stirred room temperature for 18 hours and was then filtered, washing with dichloromethane, and the filtrate concentrated in vacuo. The residue was then purified using an SCX ion exchange cartridge (Varian bond-elute) eluting with methanol followed by ammonia (0.5M to 2M in methanol). The appropriate fractions were combined and reduced in vacuo to afford a crude product which was purified further by trituration with methanol to afford the desired product D37. MS (ES+) m/e 490/492 [M+H]+.
後処理
- filtrationwas then filtered
- washwashing with dichloromethane
- concentrationthe filtrate concentrated in vacuo
- customThe residue was then purified
- washan SCX ion exchange cartridge (Varian bond-elute)
- washeluting with methanol
- customto afford a crude product which
- customwas purified further by trituration with methanol
出典と根拠
- ORDレコード
- ord-147463fb8f954a189b7f350b41a72b2c
- 出典データセット
- uspto-grants-2008_06
- 特許番号
- US07381728B2
関連ノート
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