Hydrochloric Acid → HCID 86680362, compound

HRID 83525Notes

Reaction equation

HRID 83525 reaction equation
C(OC(=O)[NH:7][CH2:8][C@@H:9]([NH:33]C(OC(C)(C)C)=O)[C:10](=[O:32])[NH:11][C:12]1[CH:16]=[C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([CH2:23][CH2:24][CH3:25])[CH:18]=2)[N:14]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[N:13]=1)(C)(C)C.[ClH:42]>O1CCOCC1>[ClH:42].[ClH:42].[NH2:33][C@H:9]([CH2:8][NH2:7])[C:10]([NH:11][C:12]1[CH:16]=[C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([CH2:23][CH2:24][CH3:25])[CH:18]=2)[N:14]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[N:13]=1)=[O:32]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 71287849HCID 71287849, compound

Product 1

HCID 86680362HCID 86680362, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

To a solution of [(R)-2-tert-butoxycarbonylamino-2-[1-phenyl-5-(3-propylphenyl)-1H-pyrazol-3-ylcarbamoyl]ethyl]carbamic acid tert-butyl ester (328 mg) in 1,4-dioxane (3 ml) was added a 4M solution of hydrogen chloride in 1,4-dioxane (3 ml) at room temperature, and the mixture was stirred for 2 hours. This reaction solution was concentrated, and then n-hexane (4 ml) was added thereto, and the mixture was stirred. The insoluble substance was collected by filtration, washed with n-hexane, and dried under reduced pressure to give the titled compound (181 mg).

Workup

  1. concentrationThis reaction solution was concentrated
  2. additionn-hexane (4 ml) was added
  3. stirringthe mixture was stirred
  4. filtrationThe insoluble substance was collected by filtration
  5. washwashed with n-hexane
  6. customdried under reduced pressure

Sources & evidence

ORD record
ord-6c2e55e5135a4bbda15edba2497a37f4
Source dataset
uspto-grants-2014_09
Patent number
US08846746B2

Reaction notes

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