Hydrochloric Acid → HCID 67130408, compound

HRID 547371Notes

Reaction equation

HRID 547371 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:18]3[CH:19]=[C:20]([F:24])[CH:21]=[C:22]([F:23])[C:17]=3[O:16][N:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:25].O1CCOCC1>C(Cl)Cl>[ClH:25].[F:24][C:20]1[CH:21]=[C:22]([F:23])[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

5

Reactant 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 59252333HCID 59252333, compound

Product 1

HCID 67130408HCID 67130408, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

4-(5,7-Difluoro-benzo[d]isoxazol-3-yl)-piperazine-1-carboxylic acid tert-butyl ester (1.69 g, 5.0 mmol) was dissolved in CH2Cl2 (30 ml) and 4 N HCl in dioxane (24.9 ml, 100 mmol) was slowly added. The resulting mixture was stirred over night at r.t. After dilution with iPr2O the product was collected by filtration and washed with one portion of iPr2O before drying it under high vacuum at 50° C. to obtain 1.35 g (98%) as a white solid. m/z=240.1 ([M+H]+).

Workup

  1. filtrationAfter dilution with iPr2O the product was collected by filtration
  2. washwashed with one portion of iPr2O
  3. custombefore drying it under high vacuum at 50° C.
  4. customto obtain 1.35 g (98%) as a white solid

Sources & evidence

ORD record
ord-fdb4e0c8818c4b5f967a402273484aa1
Source dataset
uspto-grants-2011_05
Patent number
US07939535B2

Reaction notes

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