Ethanol → HCID 11280803, compound

HRID 2251872Notes

Reaction equation

HRID 2251872 reaction equation
[C:1]1([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH:6]=[CH:5][C:4]([NH:7][CH2:8][C:9]2C(C(N(C(C)C)C(C)C)=O)=[C:13]([NH:24][CH2:25][C:26]3[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=3)[N:12]=[CH:11][CH:10]=2)=[CH:3][CH:2]=1.[CH3:38][CH2:39][OH:40]>Cl>[C:1]1([C:32]2[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=2)[CH:2]=[CH:3][C:4]([N:7]2[CH2:8][C:9]3[CH:10]=[CH:11][N:12]=[C:13]([NH:24][CH2:25][C:26]4[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=4)[C:38]=3[C:39]2=[O:40])=[CH:5][CH:6]=1

Participants

4

Reactant 2

HCID 702EthanolHCID 69033243HCID 69033243, compound

Product 1

HCID 11280803HCID 11280803, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

A solution of 4-(biphenyl-4-ylaminomethyl)-N,N-diisopropyl-2-[(pyridin-4-ylmethyl)-amino]-nicotinamide (13 mg, 0.026 mmol, Step C) in absolute EtOH (3 mL) and HCl (12 N, 1 mL) was heated to reflux for 2 days, then concentrated in vacuo. The crude material was dissolved in 1:1 DMSO to MeOH (2 mL) and purified by reverse phase HPLC (10-95% CH3CN in H2O). MS (ES+): 393.2 (M+H)+.

Workup

  1. temperatureto reflux for 2 days
  2. concentrationconcentrated in vacuo
  3. dissolutionThe crude material was dissolved in 1:1 DMSO to MeOH (2 mL)
  4. custompurified by reverse phase HPLC (10-95% CH3CN in H2O)

Sources & evidence

ORD record
ord-bca8e7cfed894db68bd3075cc224fcca
Source dataset
uspto-grants-2008_01
Patent number
US07320992B2

Reaction notes

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