Hydrochloric Acid → HCID 69796047, compound

HRID 1830050Notes

Reaction equation

HRID 1830050 reaction equation
[CH3:1][C:2]1([C:45]([F:48])([F:47])[F:46])[CH2:7][C:6]([C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][N:13]3[C:21]([C:24]([N:26]4[CH2:31][CH2:30][N:29](C(OC(C)(C)C)=O)[CH2:28][CH2:27]4)=[O:25])=[CH:22][CH:23]=[C:12]3[CH2:11]2)=[O:9])=[CH:5][CH:4]=[C:3]1[C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1.C(OCC)(=O)C.[ClH:55]>C(OCC)C>[ClH:55].[CH3:1][C:2]1([C:45]([F:47])([F:46])[F:48])[CH2:7][C:6]([C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][N:13]3[C:21]([C:24]([N:26]4[CH2:27][CH2:28][NH:29][CH2:30][CH2:31]4)=[O:25])=[CH:22][CH:23]=[C:12]3[CH2:11]2)=[O:9])=[CH:5][CH:4]=[C:3]1[C:39]1[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 86587479HCID 86587479, compound

Product 1

HCID 69796047HCID 69796047, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

The 4-[[10,11-dihydro-10-[[2-methyl-2-(trifluoromethyl)[1,1-biphenyl]-4-yl]carbonyl]-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl]carbonyl]-1-piperazinecarboxylic acid, tert-butyl ester of Step B (0.85 g, 1.29 mmol) was then added in one portion to stirred ethyl acetate (10 mL) saturated with hydrogen chloride gas at 0° C. The reaction mixture was stirred for 90 minutes under anhydrous conditions. A precipitate formed after several minutes. The reaction was then warmed to room temperature and diluted with diethyl ether. The precipitated product was collected by filtration and dried under high vacuum to provide 0.65 g of the desired title compound hydrochloride salt as an off-white foam.

Workup

  1. customA precipitate formed after several minutes
  2. filtrationThe precipitated product was collected by filtration
  3. customdried under high vacuum

Sources & evidence

ORD record
ord-138fb63884e1421a9fc127ee6e7c38ba
Source dataset
uspto-grants-2006_06
Patent number
US07064120B2

Reaction notes

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