Sodium Hydroxide → HCID 67003507, compound

HRID 2362659Notes

Reaction equation

HRID 2362659 reaction equation
[Cl:1][C:2]1[C:3]([C:25]2[S:29][C:28]([C:30]3([O:34][CH2:35][O:36][CH3:37])[CH2:33][CH2:32][CH2:31]3)=[N:27][CH:26]=2)=[C:4]2[CH:10]=[C:9]([C:11]([O:13]C)=[O:12])[N:8](S(C3C=CC(C)=CC=3)(=O)=O)[C:5]2=[N:6][CH:7]=1.[OH-].[Na+]>CO>[Cl:1][C:2]1[C:3]([C:25]2[S:29][C:28]([C:30]3([O:34][CH2:35][O:36][CH3:37])[CH2:33][CH2:32][CH2:31]3)=[N:27][CH:26]=2)=[C:4]2[CH:10]=[C:9]([C:11]([OH:13])=[O:12])[NH:8][C:5]2=[N:6][CH:7]=1

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 67003656HCID 67003656, compound

Product 1

HCID 67003507HCID 67003507, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
75 °C

Procedure

A suspension of Example 46A (0.134 g, 0.238 mmol) in methanol (2.5 mL) was treated with 2 M aqueous sodium hydroxide solution (0.714 mL, 1.19 mmol). The reaction was heated at 75° C. for 40 minutes, cooled to ambient temperature, and concentrated under reduced pressure. The residue was suspended in water (2 mL), and the pH adjusted to ˜4 with 1 N aqueous HCl solution. The suspension was filtered, and the solid collected was washed with water and dried in a vacuum oven at 60° C. to provide the title compound. ESI(+) m/z 393.9 [M+H]+.

Workup

  1. temperaturecooled to ambient temperature
  2. concentrationconcentrated under reduced pressure
  3. filtrationThe suspension was filtered
  4. customthe solid collected
  5. washwas washed with water
  6. customdried in a vacuum oven at 60° C.

Sources & evidence

ORD record
ord-912d20ef24d34be6bec35065226e661d
Source dataset
uspto-grants-2014_04
Patent number
US08691810B2

Reaction notes

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