tert-Butanol → 3-(4-Chloro-phenyl)-isothiazole-4-carboxylic acid tert-butyl ester
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:12]([C:13]([OH:15])=[O:14])=[CH:11][S:10][N:9]=2)=[CH:4][CH:3]=1.[CH3:16][C:17](O)([CH3:19])[CH3:18].CCN=C=NCCCN(C)C>CN(C1C=CN=CC=1)C.C(Cl)Cl>[C:17]([O:14][C:13]([C:12]1[C:8]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)=[N:9][S:10][CH:11]=1)=[O:15])([CH3:19])([CH3:18])[CH3:16]参加物
6
実験手順
To a mixture of 7 (3.35 g), DMAP (1.7 g) and tBuOH (5.2 g) in CH2Cl2 (50 ml) is added 3.2 g of EDCI and the clear solution is stirred over the weekend. Additional CH2Cl2 (100 ml) is added and the mixture is washed with 1N HCl (2×150 ml), sat. NaHCO3 (150 ml), brine (150 ml), dried and concentrated. This afforded 3.75 g of 8 as a pale yellow oil.
後処理
- washthe mixture is washed with 1N HCl (2×150 ml), sat. NaHCO3 (150 ml), brine (150 ml)
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-67fd5616b4144d0ca26758dc4ccd024f
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08377953B2
反応ノート
読み込み中…