Sodium Hydroxide → HCID 85960732, compound

HRID 1764119Notes

Reaction equation

HRID 1764119 reaction equation
Cl.[NH2:2][OH:3].[OH-].[Na+].[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[O:14][CH2:13][CH2:12][C:11]2=O>O.C(O)C>[CH3:6][O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[O:14][CH2:13][CH2:12][C:11]2=[N:2][OH:3]

Participants

6

Reactant 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 46121686-methoxy-3,4-dihydro-2H-1-benzopyran-4-one

Product 1

HCID 85960732HCID 85960732, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

A solution of 140 g (2.02 mole) of hydroxylamine hydrochloride in 630 ml of water, contained in a 3-l Erlenmeyer flask, was treated with 560 ml of 10% NaOH, and a solution of 250 g (1.40 mole) of 6-methoxy-4-chromanone in 560 ml of ethanol, all with rapid stirring. The reaction mixture was heated to boiling over 15 min., and continued to boil for 5 min. The mixture was stirred rapidly at room temperature for 3 hrs., refrigerated overnight and filtered. A white crystalline solid was washed with 1-l of water and air dried for 3 days; m.p. 120°-121°, Yield: 266 g (99%).

Workup

  1. temperatureThe reaction mixture was heated
  2. waitto boil for 5 min
  3. filtration, refrigerated overnight and filtered
  4. washA white crystalline solid was washed with 1-l of water and air
  5. customdried for 3 days

Sources & evidence

ORD record
ord-035518c17ccc4304b08c3f454f1eac94
Source dataset
uspto-grants-1978_09
Patent number
US04115407

Reaction notes

Loading…