Sodium Methoxide → HCID 13225516, compound

HRID 464195Notes

Reaction equation

HRID 464195 reaction equation
Cl[C:2]1[N:3]=[CH:4][C:5]2[CH2:6][N:7]=[C:8]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[C:9]3[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:10]=3[C:11]=2[N:12]=1.[CH3:25][O-:26].[Na+]>CO>[Cl:17][C:15]1[CH:14]=[CH:13][C:10]2[C:11]3[N:12]=[C:2]([O:26][CH3:25])[N:3]=[CH:4][C:5]=3[CH2:6][N:7]=[C:8]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[C:9]=2[CH:16]=1

Participants

4

Reactant 2

HCID 10942334Sodium MethoxideHCID 13225515HCID 13225515, compound

Product 1

HCID 13225516HCID 13225516, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To 25 ml of methanol was added 1.0 g (0.0279 mol) of 2,9-dichloro-7-(2-fluorophenyl)-5H-pyrimido[5,4-d][2]benzazepine and 0.18 g (0.00335 mol) of sodium methoxide. The reaction was stirred for 18 hr, and evaporated to dryness. The solid was dissolved in 50 ml of dichloromethane and washed with 40 ml of water, dried and evaporated to dryness. The oil was crystallized and recrystallized from ether/petrol and then from ether to give white prisms, mp 137°-141° C.

Workup

  1. customevaporated to dryness
  2. dissolutionThe solid was dissolved in 50 ml of dichloromethane
  3. washwashed with 40 ml of water
  4. customdried
  5. customevaporated to dryness
  6. customThe oil was crystallized
  7. customrecrystallized from ether/petrol
  8. customfrom ether to give white prisms, mp 137°-141° C.

Sources & evidence

ORD record
ord-09393365e13b4cac87328bbb97ef41f2
Source dataset
uspto-grants-1985_10
Patent number
US04546183

Reaction notes

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