Methyl iodide → HCID 19976097, compound

HRID 1450465Notes

Reaction equation

[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH2:10][C:9]([CH3:13])([CH3:12])[CH2:8][C:7]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=3)([OH:14])[C:6]=2[CH:21]=1.[H-].[Na+].[CH3:24]I>CN(C=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH2:10][C:9]([CH3:13])([CH3:12])[CH2:8][C:7]([O:14][CH3:24])([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=3)[C:6]=2[CH:21]=1

Participants

Conditions

Temperature: 80 °C

Procedure

A solution of 7-bromo-3,3-dimethyl-5-(2-pyridyl)-benzoxepin-5-ol (5 g, 0.014 mol) in anhydrous DMF (50 ml) is added dropwise to a suspension of sodium hydride (50% dispersed in oil, 0.8 g, 0.0168 mol) in anhydrous DMF (25 ml), the temperature rises to 88° C., stirring is continued for 1 hour and the reaction mixture is maintained at 80° C. A solution of methyl iodide (1.9 g, 0.014 mol) in anhydrous DMF (10 ml) is then added dropwise at 25° C.

Workup

customrises to 88° C.

Sources & evidence

ORD record: ord-e832a9a3acd642ceba27deb83d89f06f
Source dataset: uspto-grants-1997_02
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05602152

Reaction notes

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