Potassium Carbonate → HCID 18320759, Verbindung

HRID 1699529

Reaktionsgleichung

[C:1]([C:3]1[N:4]([CH2:28][C:29]2[CH:34]=[CH:33][C:32]([O:35][CH3:36])=[CH:31][C:30]=2[O:37][CH3:38])[C:5](=[O:27])[N:6]([C:17]2[C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[N:19](C)[CH:18]=2)[C:7]=1[C:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[NH:10][CH:9]=1)#[N:2].[CH3:39][S:40]([O:43][CH2:44][CH2:45][CH2:46]OS(C)(=O)=O)(=[O:42])=[O:41].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:39][S:40]([O:43][CH2:44][CH2:45][CH2:46][N:10]1[C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8]([C:7]2[N:6]([C:17]3[C:25]4[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=4)[NH:19][CH:18]=3)[C:5](=[O:27])[N:4]([CH2:28][C:29]3[CH:34]=[CH:33][C:32]([O:35][CH3:36])=[CH:31][C:30]=3[O:37][CH3:38])[C:3]=2[C:1]#[N:2])=[CH:9]1)(=[O:42])=[O:41]

Komponenten

Reaktionsbedingungen

Temperatur: 70 °C

Versuchsvorschrift

To a solution 0.15 g (0.298 mmol) of the product from step b) in 2 ml of DMF was 0.40 g (1.72 mmol) of 1,3-propandiol bismethansulfonate and 0.50 g (3.62 mmol) of K2CO3. The mixture was stirred at 70° C. overnight and partitioned between EtOAc and water. The organic phase was washed with water and brine and finally evaporated. The residue was purified by chromatography on silica furnishing 0.11 g (59%) of the sub-title compound.

Aufarbeitung

custompartitioned between EtOAc and water
washThe organic phase was washed with water and brine
customfinally evaporated
customThe residue was purified by chromatography on silica furnishing 0.11 g (59%) of the sub-title compound

Quellen und Nachweise

ORD-Eintrag: ord-8490e5a0de73423d845d5d859fab2c15
Quelldatensatz: uspto-grants-2002_02
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06346625B1

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