HCID 20292528, compound → HCID 23344997, compound

HRID 1856434Notes

Reaction equation

HRID 1856434 reaction equation
C([O:3][P:4]1(=[O:14])[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH:6]([CH3:13])[O:5]1)C>O>[OH:14][P:4]1(=[O:3])[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH:6]([CH3:13])[O:5]1

Participants

3

Reactant 1

HCID 20292528HCID 20292528, compound

Product 1

HCID 23344997HCID 23344997, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

The 1-ethoxy-3-methyl-1,3-dihydro-2,1-benzoxaphosphole-1-oxide was added to 25 ml. of water and then heated on a steam bath for 1 hour. The reaction mixture was cooled, washed with chloroform and taken to dryness under vacuum to yield a clear oil which crystallized upon scratching. Recrystallization from acetone-ether yielded 1-hydroxy-3-methyl-1,3-dihydro-2,1-benzoxaphosphole-1-oxide as a white powder. A second crop was obtained from the filtrate to give a total yield of 2.4 g (67% yield) of 1-hydroxy-3-methyl-1,3-dihydro-2,1-benzoxaphosphole-1-oxide having a melting point of 148°-149° C. and the following analysis:

Workup

  1. temperatureThe reaction mixture was cooled
  2. washwashed with chloroform
  3. customto yield a clear oil which
  4. customcrystallized
  5. customRecrystallization from acetone-ether

Sources & evidence

ORD record
ord-c523e8a434894947ae487f6aa47f5d0e
Source dataset
uspto-grants-1980_08
Patent number
US04219510

Reaction notes

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