Hydrochloric Acid → HCID 54670607, compound

HRID 449282Notes

Reaction equation

HRID 449282 reaction equation
[F:1][C:2]1[CH:7]=[C:6]([C:8]2[N:13]=[C:12]3[N:14]([CH2:17][C:18]4[CH:19]=[C:20]5[C:25](=[CH:26][CH:27]=4)[N:24]=[CH:23][CH:22]=[CH:21]5)[N:15]=[N:16][C:11]3=[CH:10][CH:9]=2)[CH:5]=[CH:4][C:3]=1[NH:28][CH2:29][CH2:30][C:31]([O:33]C)=[O:32].[OH-].[Li+].Cl>CO.O>[F:1][C:2]1[CH:7]=[C:6]([C:8]2[N:13]=[C:12]3[N:14]([CH2:17][C:18]4[CH:19]=[C:20]5[C:25](=[CH:26][CH:27]=4)[N:24]=[CH:23][CH:22]=[CH:21]5)[N:15]=[N:16][C:11]3=[CH:10][CH:9]=2)[CH:5]=[CH:4][C:3]=1[NH:28][CH2:29][CH2:30][C:31]([OH:33])=[O:32]

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 66994954HCID 66994954, compound

Product 1

HCID 54670607HCID 54670607, compoundYield 102.7%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

To a solution of example 57 (0.080 g, 0.165 mmol) in methanol (0.8 ml), lithium hydroxide (0.064 g, 1.54 mmol) in water (0.8 ml) was added and stirred at RT. After 12 h, pH was adjusted to ca. 7.5 using 0.5N HCl and the solid precipitated was filtered, washed with ethyl acetate and petroleum ether and dried under vacuum to afford the title compound as pale green solid (0.075 g, 68%). M.P.: 132-135° C.

Workup

  1. customthe solid precipitated
  2. filtrationwas filtered
  3. washwashed with ethyl acetate and petroleum ether
  4. customdried under vacuum

Sources & evidence

ORD record
ord-97118141edbf4e7bb6bf37e029de6d46
Source dataset
uspto-grants-2013_07
Patent number
US08481739B2

Reaction notes

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