Hydrochloric Acid → HCID 54735555, compound

HRID 1963089Notes

Reaction equation

HRID 1963089 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]([C:16]2[N:20]3[N:21]=[CH:22][C:23]([OH:25])=[CH:24][C:19]3=[C:18]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:17]=2[CH2:32][C:33]2[CH:38]=[CH:37][CH:36]=[C:35]([F:39])[C:34]=2[CH3:40])=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl.O1CCOCC1>C(Cl)Cl>[F:39][C:35]1[C:34]([CH3:40])=[C:33]([CH:38]=[CH:37][CH:36]=1)[CH2:32][C:17]1[C:18]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[C:19]2[CH:24]=[C:23]([OH:25])[CH:22]=[N:21][N:20]2[C:16]=1[C:14]([N:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1)=[O:15]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 67773564HCID 67773564, compound

Product 1

HCID 54735555HCID 54735555, compoundYield 82.1%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

The compound of step 3 (0.109 g, 0.20 mmol) was dissolved in 3 ml of anhydrous DCM and a 4 M solution of hydrogen chloride in dioxane (1.0 ml, 4.0 mmol) was added. After stirring at room temperature overnight, the mixture was evaporated to dryness under reduced pressure. The obtained solid was triturated several times with diethyl ether and dried in vacuo at 55° C. to give 0.073 g of the title compound in the form of [6-(3-fluoro-2-methyl-benzyl)-3-hydroxy-5-phenyl-pyrrolo[1,2-b]pyridazin-7-yl]-piperazin-1-yl-methanone hydrochloride as a greenish-yellow solid with the following characteristics:

Workup

  1. customthe mixture was evaporated to dryness under reduced pressure
  2. customThe obtained solid was triturated several times with diethyl ether
  3. customdried in vacuo at 55° C.

Sources & evidence

ORD record
ord-deed92f4fff145d49b33c552486d6952
Source dataset
uspto-grants-2013_04
Patent number
US08415336B2

Reaction notes

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