Sodium Hydroxide → HCID 22598944, compound

HRID 2252466Notes

Reaction equation

HRID 2252466 reaction equation
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[NH:7][CH2:8][CH2:9][CH2:10][N:11]1[C:19]2[C:14](=[CH:15][C:16]([C:20]([O:22]CC)=[O:21])=[CH:17][CH:18]=2)[CH:13]=[N:12]1.[OH-].[Na+]>C(O)C.O>[N:3]1[CH:4]=[CH:5][CH:6]=[N:1][C:2]=1[NH:7][CH2:8][CH2:9][CH2:10][N:11]1[C:19]2[C:14](=[CH:15][C:16]([C:20]([OH:22])=[O:21])=[CH:17][CH:18]=2)[CH:13]=[N:12]1

Participants

5

Procedure

The product of step A (510 mg, 1.16 mmol) was dissolved in ethanol (50 mL) and sodium hydroxide (6.5 mL of a 1N solution, 6.5 mmol) added. The solution was heated at reflux for 1.5 hours, diluted with water (45 mL), and the ethanol removed under vacuum. The solution was acidified to pH=3 with 1N HCl (˜7 mL) with stirring. The resulting solids were filtered, washed with water, and dried under vacuum to afford the product (308 mg, 89%).

Workup

  1. temperatureThe solution was heated
  2. temperatureat reflux for 1.5 hours
  3. customthe ethanol removed under vacuum
  4. filtrationThe resulting solids were filtered
  5. washwashed with water
  6. customdried under vacuum

Sources & evidence

ORD record
ord-719e1ee9fd6f4616ba9459aa6b0cf024
Source dataset
uspto-grants-2008_01
Patent number
US07321045B2

Reaction notes

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