Hydrochloric Acid → HCID 20402705, compound

HRID 1995097Notes

Reaction equation

HRID 1995097 reaction equation
[C:1]([C:9]1[C:10]([NH:16][C:17](=[O:21])[CH2:18][NH:19][OH:20])=[CH:11][N:12]([CH3:15])[C:13]=1[CH3:14])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:22]>C(O)(C)C>[Cl-:22].[OH:20][N:19]1[CH:1]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:9]2=[C:13]([CH3:14])[N:12]([CH3:15])[CH:11]=[C:10]2[NH2+:16][C:17](=[O:21])[CH2:18]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 20402696HCID 20402696, compound

Product 1

HCID 20402705HCID 20402705, compound

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Conditions

Temperature
0 °C

Procedure

The compound of example 1 (79.4 g) was suspended in isopropanol containing 2.1% of HCl (3700 ml) and refluxed for 2 hours with stirring. The reaction mixture was then cooled to 0° C. and a first crop (61 g) of the compound of the title which crystallized out was recovered by filtration. A second crop (9 g) was obtained by concentrating the mother liquors to a small volume. M.p. 220°-223° C. with decomposition.

Workup

  1. temperaturerefluxed for 2 hours
  2. customa first crop (61 g) of the compound of the title which crystallized out
  3. filtrationwas recovered by filtration
  4. customA second crop (9 g) was obtained
  5. concentrationby concentrating the mother liquors to a small volume

Sources & evidence

ORD record
ord-bd5492f3009a46218af7d6f893f7bc3a
Source dataset
uspto-grants-1983_09
Patent number
US04402970

Reaction notes

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