Lithium iodide → HCID 20135080, compound

HRID 580393Notes

Reaction equation

HRID 580393 reaction equation
[I-].[Li+].CO[C:5]([C:7]1(C)[CH:13]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[O:20][CH3:21])[CH2:12][C:11]2[CH:22]=[C:23]([C:26]([F:29])([F:28])[F:27])[CH:24]=[CH:25][C:10]=2[NH:9][C:8]1=[O:30])=O>N1C=CC=CC=1.C(OCC)(=O)C>[CH3:21][O:20][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[CH:13]1[CH2:12][C:11]2[CH:22]=[C:23]([C:26]([F:27])([F:28])[F:29])[CH:24]=[CH:25][C:10]=2[NH:9][C:8](=[O:30])[CH:7]1[CH3:5]

Participants

5

Reactant 2

HCID 66321Lithium iodideHCID 20135073HCID 20135073, compound

Product 1

HCID 20135080HCID 20135080, compoundYield 100%

Reagents, catalysts & solvents 2

HCID 1049PyridineCatalystHCID 8857Ethyl AcetateSolvent

Procedure

Lithium iodide (5.26 g; 39.3 mmole) was added to 1,3,4,5-tetrahydro-3-(methoxycarbonyl)-4-(methoxyphenyl)-3-methyl-7-(trifluoromethyl)-2H-1-benzazepin-2-one (4.00 g; 9.82 mmole) in pyridine (40 ml) (five drops of water were added) and the mixture was refluxed with stirring for 8.5 hours. The solution was dissolved in ethyl acetate and washed with 1N hydrochloric acid (three times). The organic layer was dried (magnesium sulfate) and concentrated giving 3.43 g of the title compound as a solid.

Workup

  1. temperaturethe mixture was refluxed
  2. washwashed with 1N hydrochloric acid (three times)
  3. dry with materialThe organic layer was dried (magnesium sulfate)
  4. concentrationconcentrated

Sources & evidence

ORD record
ord-d77f003740b14994b8c78caad6f61580
Source dataset
uspto-grants-1988_06
Patent number
US04752645

Reaction notes

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