C[O-].[Na+].[OH:4][C:5]1[CH:15]=[CH:14][C:8]2[NH:9][C:10](=[O:13])[CH2:11][S:12][C:7]=2[CH:6]=1.[NH:16]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[C:18]([CH:25]=O)=[CH:17]1>CN(C=O)C>[OH:4][C:5]1[CH:15]=[CH:14][C:8]2[NH:9][C:10](=[O:13])[C:11](=[CH:25][C:18]3[C:19]4[C:24](=[CH:23][CH:22]=[CH:21][CH:20]=4)[NH:16][CH:17]=3)[S:12][C:7]=2[CH:6]=1Sodium methoxide (0.54 g, 10 mmol) was added in one portion to a solution of 7-hydroxy-2H-1,4-benzothiazin-3(4H)-one (0.91 g, 5 mmol) and indole-3-carboxaldehyde (1.09 g, 7.5 mmol) in dry DMF (5 ml). The mixture was heated at 140° C. for 48 h, allowed to cool and poured into ice water (60 ml). The solid was collected by filtration. The filtrate was acidified to pH=2 with 10% hydrochloric acid and the precipitated solid was collected by filtration. Both precipitates were put together, boiled with toluene and filtered hot to give a solid which was purified by silica gel chromatography using a gradient of (9:1) to (8:2) n-hexane/ethanol as the mobile phase.
Wird geladen…
