Methylamine → HCID 13225524, compound

HRID 464542Notes

Reaction equation

HRID 464542 reaction equation
[CH3:1][NH2:2].C([O:5][C:6](=O)[CH2:7][C:8]1[N:9]=[CH:10][C:11]2[CH2:12][N:13]=[C:14]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[F:30])[C:15]3[CH:22]=[C:21]([Cl:23])[CH:20]=[CH:19][C:16]=3[C:17]=2[N:18]=1)C>C(O)C>[Cl:23][C:21]1[CH:20]=[CH:19][C:16]2[C:17]3[N:18]=[C:8]([CH2:7][C:6]([NH:2][CH3:1])=[O:5])[N:9]=[CH:10][C:11]=3[CH2:12][N:13]=[C:14]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[F:30])[C:15]=2[CH:22]=1

Participants

4

Reactant 2

HCID 6329MethylamineHCID 13225522HCID 13225522, compound

Product 1

HCID 13225524HCID 13225524, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Methylamine was bubbled into a solution of 2.6 g (6.34 mmol) of 9-chloro-7-(2-fluorophenyl)-5H-pyrimido[5,4-d][2]benzazepine-2-acetic acid ethylester in 60 ml of ethanol for 10 min. After standing for 18 hr, the reaction was evaporated and the residue was partitioned between 75 ml of dichloromethane and 50 ml of water. The organic layer was dried and evaporated. The residue was crystallized and then recrystallized from dichloromethane/ether to give white rods, mp 175°-177° C.

Workup

  1. customthe reaction was evaporated
  2. customthe residue was partitioned between 75 ml of dichloromethane and 50 ml of water
  3. customThe organic layer was dried
  4. customevaporated
  5. customThe residue was crystallized
  6. customrecrystallized from dichloromethane/ether
  7. customto give white rods, mp 175°-177° C.

Sources & evidence

ORD record
ord-b69e0fcadd914965975c7b9813663df5
Source dataset
uspto-grants-1985_10
Patent number
US04547581

Reaction notes

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