Hydrochloric Acid → HCID 66634061, compound

HRID 1750065Notes

Reaction equation

HRID 1750065 reaction equation
Cl.[Cl:2][C:3]1[C:8]([Cl:9])=[CH:7][CH:6]=[CH:5][C:4]=1[N:10]1[CH2:16][CH2:15][CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][CH2:11]1>CCOC(C)=O>[ClH:2].[Cl:2][C:3]1[C:8]([Cl:9])=[CH:7][CH:6]=[CH:5][C:4]=1[N:10]1[CH2:16][CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 66634155HCID 66634155, compound

Product 1

HCID 66634061HCID 66634061, compoundYield 183.7%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

Excess HCl in EtOAc was added dropwise to a solution of intermediate 1 (4.0 g, 11.6 mmol) in EtOAc and the reaction mixture was stirred at rt for 1.5 h. The reaction mixture was filtered to give 1-(2,3-dichlorophenyl)-1,4-diazepane hydrochloride salt (intermediate 2) (3.0 g, 90%) as a white solid. HPLC: 99%, RT 2.108 min. MS (ESI) m/z 245.0 [M+H]+. mp: 186-187° C.

Workup

  1. filtrationThe reaction mixture was filtered

Sources & evidence

ORD record
ord-e7701ba7c3d0468f99855f193e8c751b
Source dataset
uspto-grants-2015_10
Patent number
US09156822B2

Reaction notes

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