Water → HCID 178439942, compound

HRID 373615Notes

Reaction equation

HRID 373615 reaction equation
[CH3:1][N:2]1[C:6]2[N:7]=[C:8]([CH2:47][CH2:48][CH3:49])[N:9]([CH2:10][C:11]3[CH:16]=[CH:15][C:14]([C:17]4[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=4[C:23]4[N:27](C(C5C=CC=CC=5)(C5C=CC=CC=5)C5C=CC=CC=5)[N:26]=[N:25][N:24]=4)=[CH:13][CH:12]=3)[C:5]=2[C:4]([CH3:50])=[N:3]1.O>CC(O)=O>[CH3:1][N:2]1[C:6]2[N:7]=[C:8]([CH2:47][CH2:48][CH3:49])[N:9]([CH2:10][C:11]3[CH:12]=[CH:13][C:14]([C:17]4[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=4[C:23]4[NH:24][N:25]=[N:26][N:27]=4)=[CH:15][CH:16]=3)[C:5]=2[C:4]([CH3:50])=[N:3]1

Participants

4

Reactant 2

HCID 962WaterHCID 20093428HCID 20093428, compound

Product 1

HCID 178439942HCID 178439942, compoundYield 68%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

The material prepared in Step E (160 mg, 0.24 mmol) was dissolved in glacial HOAc (2.0 mL) at 50° C. and H2O was added dropwise until the solution just became cloudy (approx. 0.7 mL). The mixture was kept at 50° C. for 2 hours and then was evaporated to dryness under a stream of nitrogen. The residue so formed was purified by preparative tlc on 1000μ SiO2 plates developed with CHCl3 /MeOH/NH4OH (80:20:2) to give 67 mg (68%) of the title compound as its ammonium salt.

Workup

  1. customwas evaporated to dryness under a stream of nitrogen
  2. customThe residue so formed
  3. customwas purified by preparative tlc on 1000μ SiO2 plates

Sources & evidence

ORD record
ord-21f97e26e05248a49407bec7311b0047
Source dataset
uspto-grants-1992_11
Patent number
US05164407

Reaction notes

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