Hydrochloric Acid → HCID 18536749, compound

HRID 412076Notes

Reaction equation

HRID 412076 reaction equation
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:8]([O:12]CC)=[N:9]2)=[CH:4][C:3]=1[N:20]1[CH:24]=[C:23]([CH2:25][OH:26])[N:22]=[CH:21]1.Cl>C(O)C>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:8](=[O:12])[NH:9]2)=[CH:4][C:3]=1[N:20]1[CH:24]=[C:23]([CH2:25][OH:26])[N:22]=[CH:21]1

Participants

4

Procedure

To a solution of the compound of Example 35 (740 mg, 1.97 mmol) in ethanol (50 ml) was added concentrated hydrochloric acid (5 ml), and the mixture was refluxed for 16 hours, attaching Dean-Stark refluxing apparatus equipped with molecular sieves 4A. After cooling, the precipitated crystals were collected by filtration, washed with ethanol and then dried under reduced pressure, thereby obtaining 994 mg of title compound as light brown powder. The yield was quantitative.

Workup

  1. temperaturethe mixture was refluxed for 16 hours
  2. temperaturerefluxing apparatus
  3. temperatureAfter cooling
  4. filtrationthe precipitated crystals were collected by filtration
  5. washwashed with ethanol
  6. customdried under reduced pressure

Sources & evidence

ORD record
ord-7195fb27b75c4498809eda286eb08427
Source dataset
uspto-grants-2003_05
Patent number
US06562839B1

Reaction notes

Loading…