Sodium Hydroxide → HCID 21851255, compound

HRID 617153Notes

Reaction equation

HRID 617153 reaction equation
C([O:3][C:4]([CH:6]1[CH2:11][CH2:10][N:9]([C:12]2[N:21]=[C:20]([N:22]3[CH2:27][CH2:26][CH:25]([N:28]4[C:37](=[O:38])[C:36]5[C:31](=[CH:32][CH:33]=[C:34]([CH3:39])[CH:35]=5)[N:30]([CH3:40])[C:29]4=[O:41])[CH2:24][CH2:23]3)[C:19]3[C:14](=[CH:15][C:16]([O:44][CH3:45])=[C:17]([O:42][CH3:43])[CH:18]=3)[N:13]=2)[CH2:8][CH2:7]1)=[O:5])C.[OH-].[Na+]>CO>[C:4]([CH:6]1[CH2:11][CH2:10][N:9]([C:12]2[N:21]=[C:20]([N:22]3[CH2:23][CH2:24][CH:25]([N:28]4[C:37](=[O:38])[C:36]5[C:31](=[CH:32][CH:33]=[C:34]([CH3:39])[CH:35]=5)[N:30]([CH3:40])[C:29]4=[O:41])[CH2:26][CH2:27]3)[C:19]3[C:14](=[CH:15][C:16]([O:44][CH3:45])=[C:17]([O:42][CH3:43])[CH:18]=3)[N:13]=2)[CH2:8][CH2:7]1)([OH:5])=[O:3]

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 15871773HCID 15871773, compound

Product 1

HCID 21851255HCID 21851255, compoundYield 81%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

In 10 ml of methanol was dissolved 400 mg (0.65 mmol) of Compound 3 obtained in Example 3, and 5 ml of 2 N aqueous solution of sodium hydroxide was added to the solution, followed by heating under reflux for one hour. After cooling, the solvent was evaporated, and water and concentrated hydrochloric acid were added to the residue. The precipitated crystals were collected by filtration, and then washed with water and methanol to give 308.0 mg (yield: 81%) of Compound 4 as white crystals.

Workup

  1. additionwas added to the solution
  2. temperatureby heating
  3. temperatureunder reflux for one hour
  4. temperatureAfter cooling
  5. customthe solvent was evaporated
  6. additionwater and concentrated hydrochloric acid were added to the residue
  7. filtrationThe precipitated crystals were collected by filtration
  8. washwashed with water and methanol

Sources & evidence

ORD record
ord-79830b709b214793be8589fd04307fa0
Source dataset
uspto-grants-1999_09
Patent number
US05948784

Reaction notes

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