Hydrochloric Acid → HCID 54670607, compound

HRID 1404796Notes

Reaction equation

HRID 1404796 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-60dba7025f5947cbbb4ada5a7dbd0370
Source dataset
uspto-grants-2014_12
Patent number
US08912331B2

Reaction notes

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