Ammonium Hydroxide → 6-(Trifluoromethyl)pyridazin-3-amine

HRID 1412037Notes

Reaction equation

HRID 1412037 reaction equation
Cl[C:2]1[N:3]=[N:4][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:7]=1.[OH-].[NH4+:13]>C1COCC1>[F:9][C:8]([F:11])([F:10])[C:5]1[N:4]=[N:3][C:2]([NH2:13])=[CH:7][CH:6]=1

Participants

4

Conditions

Temperature
100 °C

Procedure

A mixture of 3-chloro-6-trifluoromethylpyridazine (1.6 g, 8.80 mmol) and ammonium hydroxide (9 mL) in THF (3 mL) was heated at 100° C. in a microwave reactor for 1 h. After this period, the reaction mixture was evaporated and the residue was extracted with dichloromethane. The combined extract was dried over with MgSO4, filtered, and evaporated under reduce pressure to afford 301a (1.3 g, 93%) as a white solid. MS-ESI: [M+H]+ 164.1

Workup

  1. waitAfter this period
  2. customthe reaction mixture was evaporated
  3. extractionthe residue was extracted with dichloromethane
  4. extractionThe combined extract
  5. dry with materialwas dried over with MgSO4
  6. filtrationfiltered
  7. customevaporated

Sources & evidence

ORD record
ord-9e9fdb0f450b452a90aeaae5586db777
Source dataset
uspto-grants-2014_12
Patent number
US08921353B2

Reaction notes

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