Hydrochloric Acid → HCID 67229718, compound

HRID 2265914Notes

Reaction equation

HRID 2265914 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:18]3[CH:19]=[C:20]([F:23])[CH:21]=[CH:22][C:17]=3[O:16][N:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:24].O1CCOCC1>ClCCl.C(OC(C)C)(C)C>[ClH:24].[F:23][C:20]1[CH:21]=[CH:22][C:17]2[O:16][N:15]=[C:14]([N:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)[C:18]=2[CH:19]=1

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 59252270HCID 59252270, compound

Product 1

HCID 67229718HCID 67229718, compound

Reagents, catalysts & solvents 2

HCID 6344DichloromethaneSolventHCID 7914Diisopropyl EtherSolvent

Procedure

4-(5-Fluoro-benzo[d]isoxazol-3-yl)-piperazine-1-carboxylic acid tert-butyl ester (22.7 g, 70.6 mmol) was dissolved in 40 ml dichloromethane and 4N HCl in dioxane (264 ml, 1.06 mol) was added. The white suspension was stirred for 16 hours at room temperature, diluted with diisopropylether and filtered. The crystals were washed with diisopropylether and dried for 1 hour at 50° C. and <20 mbar, to get the desired salt as a white solid (18.2 g, quant.) [MS: m/e=222.3 (M+H+)].

Workup

  1. filtrationfiltered
  2. washThe crystals were washed with diisopropylether
  3. customdried for 1 hour at 50° C.

Sources & evidence

ORD record
ord-25a14b352b1d48ae8eeeac6bf4ddcf0a
Source dataset
uspto-grants-2010_12
Patent number
US07858630B2

Reaction notes

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