HCID 12621061, compound → HCID 12621072, compound

HRID 330108Notes

Reaction equation

HRID 330108 reaction equation
[CH:1]12[CH2:7][CH:4]([CH:5]=[CH:6]1)[CH2:3][CH:2]2[C:8](=[O:18])[CH:9]([CH:11]1[CH2:16][CH:15]2[CH2:17][CH:12]1[CH:13]=[CH:14]2)[OH:10]>C(OCCO)C.C(O)(=O)C>[CH:12]12[CH2:17][CH:15]([CH:14]=[CH:13]1)[CH2:16][CH:11]2[C:9](=[O:10])[C:8]([CH:2]1[CH2:3][CH:4]2[CH2:7][CH:1]1[CH:6]=[CH:5]2)=[O:18]

Participants

4

Reactant 1

HCID 12621061HCID 12621061, compound

Product 1

HCID 12621072HCID 12621072, compound

Reagents, catalysts & solvents 2

HCID 176Acetic AcidSolventHCID 8076Glycol monoethyl etherSolvent

Procedure

49.9 g (204 millimoles) of VII in 130 ml of 2-ethoxyethanol and 40 ml of glacial acetic acid are heated to 105° C., while stirring. 25.0 g (53.6 millimoles) of Bi2O3 are then added all at once. After a reaction time of 2 hours, the elemental bismuth is filtered off and washed with 300 ml of chloroform. The organic phase is washed neutral with water. The solvent is stripped off and the residue subjected to fractional distillation. The product is then recrystallized from petroleum ether.

Workup

  1. filtrationAfter a reaction time of 2 hours, the elemental bismuth is filtered off
  2. washwashed with 300 ml of chloroform
  3. washThe organic phase is washed neutral with water
  4. distillationthe residue subjected to fractional distillation
  5. customThe product is then recrystallized from petroleum ether

Sources & evidence

ORD record
ord-32dd2d93a06343d1a17258e21bf24fc9
Source dataset
uspto-grants-1990_01
Patent number
US04894483

Reaction notes

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