Hydrochloric Acid → HCID 18473242, compound
Reaction equation
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][N:12]([S:15]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([OH:24])[CH:19]=2)(=[O:17])=[O:16])[CH2:11][CH2:10]1)=O)(C)(C)C>CCOC(C)=O>[ClH:1].[N:12]1([S:15]([C:18]2[CH:19]=[C:20]([OH:24])[CH:21]=[CH:22][CH:23]=2)(=[O:17])=[O:16])[CH2:11][CH2:10][NH:9][CH2:14][CH2:13]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
HCl gas was bubbled into a solution of 4-(3-hydroxy-benzenesulfonyl)-piperazine-1-carboxylic acid tert-butyl ester (2.3 g, 9.5 mmol) in EtOAc (100 mL) at −20° C. with stirring for 10 min. The solution was stoppered, stirred for 1 h, purged with Ar for 15 min, then concentrated in vacuo to the title compound as a white solid. 1H NMR (d6-DMSO) δ 8.97, br s, 1H), 7.50 (t, 1H, J=8 Hz), 7.12-7.19 (m, 2H), 3.175 (d, 2H, J=5 Hz), 3.12 (t, 2H, J=5 Hz).
Workup
- stirringstirred for 1 h
- custompurged with Ar for 15 min
- concentrationconcentrated in vacuo to the title compound as a white solid
Sources & evidence
- ORD record
- ord-654274563eaa42ccb73f24fbfe0210f8
- Source dataset
- uspto-grants-2002_07
- Patent number
- US06413964B1
Reaction notes
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