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Hydrogen chloride-ethyl acetate → HCID 66975080, compound

HRID 1022615
Notes
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Reaction equation

HRID 1022615 reaction equation
C(OC([NH:8][S:9]([NH:12][CH2:13][C@H:14]1[C@H:20]([C:21]2[CH:26]=[CH:25][C:24]([Cl:27])=[C:23]([Cl:28])[CH:22]=2)[O:19][CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15]1)(=[O:11])=[O:10])=O)(C)(C)C.C(OCC)(=O)C.Cl>C(O)C>[ClH:27].[Cl:28][C:23]1[CH:22]=[C:21]([C@@H:20]2[O:19][CH2:18][CH2:17][NH:16][CH2:15][C@H:14]2[CH2:13][NH:12][S:9]([NH2:8])(=[O:10])=[O:11])[CH:26]=[CH:25][C:24]=1[Cl:27]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 66975769HCID 66975769, compound

Product 1

HCID 66975080HCID 66975080, compoundYield 146.9%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of tert-butyl (6S,7R)-6-({[(tert-butoxycarbonyl)sulfamoyl]amino}methyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (172 mg) in ethanol (0.5 mL) was added 4.0 M hydrogen chloride-ethyl acetate solution (3 mL), and the mixture was stirred at room temperature for 2 hr. The solvent was evaporated under reduced pressure. The obtained crystals were recrystallized from ethanol-water to give the title compound (89 mg) as colorless crystals.

Workup

  1. customThe solvent was evaporated under reduced pressure
  2. customThe obtained crystals were recrystallized from ethanol-water

Sources & evidence

ORD record
ord-f543781ac2c34a4788528f1161d2ad3f
Source dataset
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08722662B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes