Hydroxyamine hydrochloride → HCID 86160832, compound

HRID 622207Notes

Reaction equation

HRID 622207 reaction equation
[Br:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[O:15][CH3:16])=O.Cl.[NH2:18][OH:19]>N1C=CC=CC=1>[Br:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[O:15][CH3:16])=[N:18][OH:19]

Participants

4

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 14097218HCID 14097218, compound

Product 1

HCID 86160832HCID 86160832, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

A solution of 20 g of (3-bromothien-2-yl) (2-methoxyphenyl)methanone in 200 g of pyridine containing 10 g of hydroxylamine hydrochloride was heated at 100° for 10 minutes and thereafter allowed to cool. After standing at room temperature for 16 hours, the solution was poured onto 600 g of ice water and the organics were extracted into ether. The combined ether solution was washed with 1N hydrochloric acid and water, and dried over anhydrous magnesium sulfate. Evaporation of the solvent under vacuum left a solid residue which was recrystallized from ether/hexane to give prisms, m.p. 129°-130° C.

Workup

  1. temperatureto cool
  2. extractionthe organics were extracted into ether
  3. washThe combined ether solution was washed with 1N hydrochloric acid and water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customEvaporation of the solvent under vacuum
  6. waitleft a solid residue which
  7. customwas recrystallized from ether/hexane
  8. customto give prisms, m.p. 129°-130° C.

Sources & evidence

ORD record
ord-1d85ed72a64342cdb545c58fb1ae790a
Source dataset
uspto-grants-1988_09
Patent number
US04769472

Reaction notes

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