Acetic Acid → HCID 178441871, compound

HRID 2259600Notes

Reaction equation

HRID 2259600 reaction equation
[CH2:1]([C:5]1[N:10]=[C:9](Cl)[C:8]([CH2:12][C:13]([O:15]CC)=[O:14])=[C:7]([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=3[C:31]([O:33]C)=[O:32])=[CH:21][CH:20]=2)[N:6]=1)[CH2:2][CH2:3][CH3:4].Cl.C(=O)(O)[O-:37].[Na+].C(O)(=O)C>O>[CH2:1]([C:5]1[N:6]=[C:7]([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=3[C:31]([OH:33])=[O:32])=[CH:21][CH:20]=2)[C:8]([CH2:12][C:13]([OH:15])=[O:14])=[C:9]([OH:37])[N:10]=1)[CH2:2][CH2:3][CH3:4]

Participants

6

Reactant 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 86749147HCID 86749147, compound

Product 1

HCID 178441871HCID 178441871, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

50 mg of the product of Example 7 were introduced into 1 ml of 6N hydrochloric acid and the mixture was heated to gentle reflux. The mixture was stirred for 2 hours 30 minutes and after cooling, the mixture was diluted with 2 ml of water. The pH was adjusted to 7-8 by the addition of sodium bicarbonate, then returned to pH 5-4 by the addition of acetic acid. The mixture was stirred for approximately 30 minutes, followed by separating, and rinsing with water to obtain 30 mg of the expected product melting approx. 220° C.

Workup

  1. temperaturethe mixture was heated to gentle reflux
  2. temperatureafter cooling
  3. stirringThe mixture was stirred for approximately 30 minutes
  4. customby separating
  5. washrinsing with water

Sources & evidence

ORD record
ord-0519ea2f074e4ed48c6fc548378283d0
Source dataset
uspto-grants-1995_12
Patent number
US05474996

Reaction notes

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