HCID 18355460, compound → HCID 18355455, compound

HRID 429337Notes

Reaction equation

HRID 429337 reaction equation
[I:1][C:2]1[CH:3]=[C:4]([CH:23]=[C:24]([I:27])[C:25]=1[OH:26])[C:5]([C:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[O:9][C:8]=1[CH2:16][CH2:17][C:18]([O:20]CC)=[O:19])=[O:6]>C(O)(=O)C.Cl>[I:27][C:24]1[CH:23]=[C:4]([CH:3]=[C:2]([I:1])[C:25]=1[OH:26])[C:5]([C:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[O:9][C:8]=1[CH2:16][CH2:17][C:18]([OH:20])=[O:19])=[O:6]

Participants

4

Conditions

Temperature
90 °C

Procedure

300 g of compound 5 are dissolved in 200 ml of acetic acid and 300 ml of 12N HCl. Stir at 90° C. for 2 hours and distill at least 400 ml of solvent. Cool to room temperature and add 1 L of water. Stir well for 2 hours and filter. Wash with water. Dry.

Workup

  1. distillationdistill at least 400 ml of solvent
  2. temperatureCool to room temperature
  3. additionadd 1 L of water
  4. stirringStir well for 2 hours
  5. filtrationfilter
  6. washWash with water
  7. customDry

Sources & evidence

ORD record
ord-d233b77f8c774155a04985245f1fd81c
Source dataset
uspto-grants-2001_11
Patent number
US06316487B1

Reaction notes

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