Thionyl Chloride → 3-(N,N-Dimethylsulfamoyl)-4-methoxybenzyl chloride
反応式
[CH3:1][N:2]([CH3:16])[S:3]([C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][C:13]=1[O:14][CH3:15])[CH2:9]O)(=[O:5])=[O:4].S(Cl)([Cl:19])=O>C(Cl)Cl>[CH3:1][N:2]([CH3:16])[S:3]([C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][C:13]=1[O:14][CH3:15])[CH2:9][Cl:19])(=[O:5])=[O:4]参加物
4
実験手順
To a solution of OBS02053 (2.33 g, 8.89 mmol) in anhydrous DCM (50 mL) was added thionyl chloride (0.97 mL, 13.34 mmol). The mixture was stirred at room temperature for 2 h and the volatiles removed in vacuo. The residue was re-dissolved and co-evaporated three times with DCM (3×20 mL) to give OBS02058 as a light-sensitive brown oil (2.07 g, 83%); 1H-NMR (270 MHz, CDCl3)=2.98 (6H, s), 3.89 (3H, s), 4.54 (2H, s), 6.94 (1H, d, J=8.4), 7.25 (1H, dd, J=2.2, 8.4), 7.40 (1H, d, J=2.2).
後処理
- customthe volatiles removed in vacuo
- dissolutionThe residue was re-dissolved
出典と根拠
- ORDレコード
- ord-36fd3da7199a4a2b8b7c77120472a4e9
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07361677B2
反応ノート
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