Sodium Methoxide → HCID 13067103, compound

HRID 1995530Notes

Reaction equation

HRID 1995530 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-8b1e3457d6c44ec2a8dc2e64691eaf14
Source dataset
uspto-grants-1983_09
Patent number
US04405518

Reaction notes

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