Sodium Carbonate → HCID 22449418, compound

HRID 2257828Notes

Reaction equation

HRID 2257828 reaction equation
[C:1]([NH:4][CH:5]1[CH2:14][C:13]2[C:8](=[C:9]([NH:17]C(=O)C)[CH:10]=[CH:11][C:12]=2[O:15][CH3:16])[C:7](=[O:21])[CH2:6]1)(=[O:3])[CH3:2].C(=O)([O-])[O-].[Na+].[Na+]>Cl>[C:1]([NH:4][CH:5]1[CH2:14][C:13]2[C:8](=[C:9]([NH2:17])[CH:10]=[CH:11][C:12]=2[O:15][CH3:16])[C:7](=[O:21])[CH2:6]1)(=[O:3])[CH3:2]

Participants

4

Conditions

Temperature
60 °C

Procedure

102 mg of the compound prepared in (4) above was charged into 20 ml of 3N hydrochloric acid aqueous solution, and the mixture was heated at 60° C. for 2 hours while stirring. After cooling to 0° C. the reaction mixture was neutralized with sodium carbonate and extracted with chloroform. The extract was dried over magnesium sulfate, and subjected to silica gil column chromatograghy using an chloroform-methanol (40:1) mixed solvent as an eluant to obtain fractions containing the target compound. The fractions were concentrated to produce 66 mg of the title compound.

Workup

  1. temperatureAfter cooling to 0° C. the reaction mixture
  2. extractionextracted with chloroform
  3. dry with materialThe extract was dried over magnesium sulfate
  4. additionmixed solvent as an eluant
  5. customto obtain fractions
  6. additioncontaining the target compound
  7. concentrationThe fractions were concentrated

Sources & evidence

ORD record
ord-24fde77c5f144559a8e19f8bcff9e045
Source dataset
uspto-grants-1997_08
Patent number
US05658920

Reaction notes

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