Hydrogen chloride-ethyl acetate → HCID 66975036, compound

HRID 1022539Notes

Reaction equation

HRID 1022539 reaction equation
[C:1]([NH:4][CH2:5][CH:6]1[CH:12]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[C:15]([Cl:20])[CH:14]=2)[O:11][CH2:10][CH2:9][N:8](C(OC(C)(C)C)=O)[CH2:7]1)(=[O:3])[NH2:2].C(OCC)(=O)C.Cl>C(O)C>[ClH:19].[Cl:20][C:15]1[CH:14]=[C:13]([CH:12]2[O:11][CH2:10][CH2:9][NH:8][CH2:7][CH:6]2[CH2:5][NH:4][C:1]([NH2:2])=[O:3])[CH:18]=[CH:17][C:16]=1[Cl:19]

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 66975736HCID 66975736, compound

Product 1

HCID 66975036HCID 66975036, compoundYield 150.4%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of tert-butyl (6RS,7SR)-6-[(carbamoylamino)methyl]-7-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (160 mg) in ethanol (0.5 mL) was added 4 N hydrogen chloride-ethyl acetate solution (3.0 mL), and the mixture was stirred at room temperature for 2 hr. The crystals obtained by concentration under reduced pressure were recrystallized from ethanol-water to give the title compound (102 mg).

Workup

  1. customThe crystals obtained by concentration under reduced pressure
  2. customwere recrystallized from ethanol-water

Sources & evidence

ORD record
ord-127b6cc121ca4a64a00f60b2634c1a56
Source dataset
uspto-grants-2014_05
Patent number
US08722662B2

Reaction notes

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