Cesium carbonate → HCID 67362631, compound

HRID 1183189Notes

Reaction equation

[CH3:1][O:2][C:3]([C:5]1[CH:9]=[C:8]([OH:10])[N:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[F:17])[N:6]=1)=[O:4].C(=O)([O-])[O-].[Cs+].[Cs+].Br[CH2:25][C:26](=[O:31])[C:27]([CH3:30])([CH3:29])[CH3:28]>CN(C=O)C>[CH3:1][O:2][C:3]([C:5]1[CH:9]=[C:8]([O:10][CH2:25][C:26](=[O:31])[C:27]([CH3:30])([CH3:29])[CH3:28])[N:7]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[F:17])[N:6]=1)=[O:4]

Participants

Conditions

Temperature: 50 °C

Procedure

200 mg (0.85 mmol) of 1-(2-fluoro-phenyl)-5-hydroxy-1H-pyrazole-3-carboxylic acid methyl ester were dissolved in 5 ml of DMF. 552 mg (1.7 mmol) of cesium carbonate and 152 mg (0.85 mmol) of 1-bromo-3,3-dimethyl-butan-2-one were added and the mixture was heated to 50° C. for 6 h. Then the mixture was filtered and the solvent removed in vacuo. The obtained crude title compound was subjected to hydrolysis without further purification.

Workup

filtrationThen the mixture was filtered
customthe solvent removed in vacuo

Sources & evidence

ORD record: ord-b6ec86607a68405d852e31427c76f1c0
Source dataset: uspto-grants-2014_03
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08664257B2

Reaction notes

Loading…