Sodium Hydroxide → HCID 66592658, compound

HRID 1091873Notes

Reaction equation

HRID 1091873 reaction equation
[F:1][CH:2]([F:25])[O:3][C:4]1[C:9]2[O:10][C:11]3[C:12](=[O:19])[N:13]([CH2:17][CH3:18])[N:14]=[CH:15][C:16]=3[C:8]=2[C:7]([C:20]([O:22]CC)=[O:21])=[CH:6][CH:5]=1.[OH-].[Na+]>CO>[F:25][CH:2]([F:1])[O:3][C:4]1[C:9]2[O:10][C:11]3[C:12](=[O:19])[N:13]([CH2:17][CH3:18])[N:14]=[CH:15][C:16]=3[C:8]=2[C:7]([C:20]([OH:22])=[O:21])=[CH:6][CH:5]=1

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 66592833Ethyl 6-difluoromethoxy-3-ethyl-4-oxo-3,4-dihydrobenzo[4,5]furo[2,3-d]pyridazine-9-carboxylate

Product 1

HCID 66592658HCID 66592658, compoundYield 88.9%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of ethyl 6-difluoromethoxy-3-ethyl-4-oxo-3,4-dihydrobenzo[4,5]furo[2,3-d]pyridazine-9-carboxylate (from step 1) (120 mg, 0.34 mmol) and sodium hydroxide (20 mg, 0.51 mmol) in methanol (20 ml) was heated to reflux temp. Progress of reaction was monitored by TLC. At the end, reaction mixture was concentrated under vacuum. Then water (50 ml) was added to reaction mixture and acidified with dilute HCl. The precipitate obtained was filtered and dried in oven. 98 mg white colored solid was obtained.

Workup

  1. temperaturewas heated
  2. temperatureto reflux temp
  3. customProgress of reaction
  4. customAt the end, reaction mixture
  5. concentrationwas concentrated under vacuum
  6. additionThen water (50 ml) was added to reaction mixture
  7. customThe precipitate obtained
  8. filtrationwas filtered
  9. customdried in oven

Sources & evidence

ORD record
ord-3b49ed99904f490daf3a09334413a5f3
Source dataset
uspto-grants-2012_03
Patent number
US08129401B2

Reaction notes

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