Hydroxyamine hydrochloride → HCID 86750165, compound

HRID 233478Notes

Reaction equation

HRID 233478 reaction equation
O=[C:2]1[C:11]2[O:10][CH2:9][CH2:8][CH2:7][C:6]=2[CH:5]=[C:4]2[O:12][CH2:13][CH2:14][CH:3]12.Cl.[NH2:16][OH:17].C([O-])(=O)C.[Na+]>C(O)C>[OH:17][N:16]=[C:2]1[C:11]2[O:10][CH2:9][CH2:8][CH2:7][C:6]=2[CH:5]=[C:4]2[O:12][CH2:13][CH:14]=[C:3]12

Participants

5

Reactant 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 22911334HCID 22911334, compound

Product 1

HCID 86750165HCID 86750165, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

27.4 g of 2,3,7,8-tetrahydro-4-oxofuro[2,3-g]benzopyran (see Preparation 1), 42 g of hydroxylamine hydrochloride and 41.9 g of sodium acetate in 288 ml of ethanol are heated at reflux for 1 hour. The solvent is evaporated off and the residue is taken up in dichloromethane and washed with water. After drying over magnesium sulphate, evaporation and then recrystallisation from ethanol, 21.85 g of the desired compound are obtained.

Workup

  1. temperatureat reflux for 1 hour
  2. customThe solvent is evaporated off
  3. washwashed with water
  4. dry with materialAfter drying over magnesium sulphate, evaporation
  5. customrecrystallisation from ethanol, 21.85 g of the desired compound
  6. customare obtained

Sources & evidence

ORD record
ord-f0fed1aa92724eaab72555487a8bd675
Source dataset
uspto-grants-1997_01
Patent number
US05593989

Reaction notes

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