Sodium Methoxide → HCID 13067103, compound

HRID 2296309Notes

Reaction equation

HRID 2296309 reaction equation
[Cl:1][C:2]1[CH:29]=[CH:28][C:5]2[C:6]3[C:7](=[C:18]([C:22](C(Cl)(Cl)Cl)=[O:23])[NH:19][C:20]=3[CH3:21])[CH2:8][N:9]=[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[F:17])[C:4]=2[CH:3]=1.[CH3:30][O-:31].[Na+]>CO>[CH3:30][O:31][C:22]([C:18]1[NH:19][C:20]([CH3:21])=[C:6]2[C:5]3[CH:28]=[CH:29][C:2]([Cl:1])=[CH:3][C:4]=3[C:10]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[F:17])=[N:9][CH2:8][C:7]=12)=[O:23]

Participants

4

Reactant 2

HCID 10942334Sodium MethoxideHCID 13067102HCID 13067102, compound

Product 1

HCID 13067103HCID 13067103, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

A mixture of 3.0 g (6.4 mmole) of 8-chloro-6-(2-fluorophenyl)-1-methyl-3-[(trichloromethyl)carbonyl]-2H,4H-pyrrolo[3,4-d][2]benzazepine, 0.5 ml (2 mmole) of a 4 M methanol solution of sodium methoxide and 100 ml of methanol was heated to 40° for 30 min. The methanol solution was concentrated at reduced pressure, and the residue was partitioned between methylene chloride and water. The methylene chloride solution was dried with anhydrous sodium sulfate and concentrated at reduced pressure to give (mp 228°-231°) tan needles. Recrystallization from methylene chloride gave fine colorless needles, mp 229°-231°.

Workup

  1. temperaturewas heated to 40° for 30 min
  2. concentrationThe methanol solution was concentrated at reduced pressure
  3. customthe residue was partitioned between methylene chloride and water
  4. dry with materialThe methylene chloride solution was dried with anhydrous sodium sulfate
  5. concentrationconcentrated at reduced pressure

Sources & evidence

ORD record
ord-e22604967064439ab02f9651a59722b9
Source dataset
uspto-grants-1984_01
Patent number
US04428879

Reaction notes

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