Methanol → HCID 13271792, compound

HRID 464583Notes

Reaction equation

HRID 464583 reaction equation
Cl[C:2]1[C:12]2[C:11]3[CH:13]=[CH:14][C:15]([Cl:17])=[CH:16][C:10]=3[C:9]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[N:8][CH2:7][C:6]=2[N:5]=[C:4]([CH3:24])[N:3]=1.[CH3:25][OH:26].C[O-].[Na+]>O1CCCC1>[Cl:17][C:15]1[CH:14]=[CH:13][C:11]2[C:12]3[C:2]([O:26][CH3:25])=[N:3][C:4]([CH3:24])=[N:5][C:6]=3[CH2:7][N:8]=[C:9]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:10]=2[CH:16]=1

Participants

5

Reactant 3

HCID 887Methanol2×HCID 10942334Sodium MethoxideHCID 132717911,9-Dichloro-3-methyl-7-phenyl-5H-pyrimido[4,5-d][2]benzazepine

Product 1

HCID 13271792HCID 13271792, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

A solution of 1.0 g (2.8 mmol) of 1,9-dichloro-3-methyl-7-phenyl-5H-pyrimido[4,5-d][2]benzazepine and 1.0 mL of a 4.2M methanol solution of sodium methoxide in 20 mL of a 1:1 mixture of methanol and tetrahydrofuran was stirred at room temperature for 1 hr. The solvent was removed at reduced pressure and the residue was triturated with water to give an off-white solid. Recrystallization from a mixture of ether and petroleum ether gave colorless prisms, mp 185°-187°.

Workup

  1. customThe solvent was removed at reduced pressure
  2. customthe residue was triturated with water
  3. customto give an off-white solid
  4. customRecrystallization
  5. additionfrom a mixture of ether and petroleum ether
  6. customgave colorless prisms, mp 185°-187°

Sources & evidence

ORD record
ord-07a012ba4dce467f9dc17eecf38bf43a
Source dataset
uspto-grants-1985_10
Patent number
US04548750

Reaction notes

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