Water → HCID 12960073, compound

HRID 1156529Notes

Reaction equation

HRID 1156529 reaction equation
Cl.[NH2:2][OH:3].[OH-].[Na+].O.[F:7][C:8]([F:20])([F:19])[C:9]1[CH:10]=[C:11]([C:15]#[C:16][C:17]#[N:18])[CH:12]=[CH:13][CH:14]=1>CO>[F:7][C:8]([F:19])([F:20])[C:9]1[CH:10]=[C:11]([C:15]2[O:3][N:2]=[C:17]([NH2:18])[CH:16]=2)[CH:12]=[CH:13][CH:14]=1

Participants

6

Reactant 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 20534845HCID 20534845, compound

Product 1

HCID 12960073HCID 12960073, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Conditions

Temperature
25 °C

Procedure

Hydroxylamine hydrochloride (1.6 grams), and sodium hydroxide (1.6 grams) were dissolved in 32 ml. of a 1:1 mixture of water and methanol at 0°-5° C. 3-(3-(Trifluoromethyl)phenyl)propiolonitrile (2.8 grams) in 10 ml. of methanol was added portionwise, and the reaction mixture was stirred overnight (about 18 hours) at 25° C. Solvent was evaporated; water was added to the residue and the product extracted with ether, washed with water, dried and evaporated, yield 1.4 grams. The identity of the desired product was confirmed by NMR.

Workup

  1. customSolvent was evaporated
  2. additionwater was added to the residue
  3. extractionthe product extracted with ether
  4. washwashed with water
  5. customdried
  6. customevaporated

Sources & evidence

ORD record
ord-8d0dac45e8504a98bdf37e5cb1112619
Source dataset
uspto-grants-1982_06
Patent number
US04336264

Reaction notes

Loading…