Hydrochloric Acid → HCID 24880030, compound

HRID 1485875Notes

Reaction equation

HRID 1485875 reaction equation
[C:1]1([C:7]2[CH:12]=[C:11]([N:13]3[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[N:10]=[N:9][C:8]=2[C:19]([F:22])([F:21])[F:20])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:23].CC(O)C>CC(=O)CC>[ClH:23].[C:1]1([C:7]2[CH:12]=[C:11]([N:13]3[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]3)[N:10]=[N:9][C:8]=2[C:19]([F:22])([F:21])[F:20])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 24880031HCID 24880031, compound

Product 1

HCID 24880030HCID 24880030, compoundYield 58%

Reagents, catalysts & solvents 1

HCID 6569Methyl Ethyl KetoneSolvent

Conditions

Temperature
50 °C

Procedure

To a solution of E1 (16 g, 51.90 mmol) in 2-butanone (400 ml) warmed to 50° C. was added dropwise, hydrochloric acid in 2-propanol (6N, 51.90 mmol). The mixture was heated at reflux temperature for 90 minutes and then stirred for 2 hours at 50° C. and further overnight at room temperature. The precipitated crystals were filtered off and dried under vacuum at 45° C., to yield E40 (10.4 g, 58%).

Workup

  1. additionwas added dropwise
  2. temperatureThe mixture was heated
  3. temperatureat reflux temperature for 90 minutes
  4. filtrationThe precipitated crystals were filtered off
  5. customdried under vacuum at 45° C.

Sources & evidence

ORD record
ord-815747cc8b5849048ed46cbff5321a60
Source dataset
uspto-grants-2016_08
Patent number
US09422296B2

Reaction notes

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