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1,2-Dichloroethane → 3-[5-Oxo-pyrrolidine-2(S)-carbonylamino]-2,3-dihydro-2-oxo-5-phenyl-1H-1,4-benzodiazepine

HRID 1458974
Notes
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Reaction equation

HRID 1458974 reaction equation
Br.[NH2:2][CH:3]1[N:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:7]2[CH:16]=[CH:17][CH:18]=[CH:19][C:6]=2[NH:5][C:4]1=[O:20].[NH4+].[NH4+].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[Ce+4].C(C(C(C([O-])=O)O)O)([O-])=O.[K+].[K+].Br.C(O)(=O)C.[NH:65]1[C:69](=[O:70])[CH2:68][CH2:67][C@H:66]1[C:71](O)=[O:72].C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.C(N(C(C)C)CC)(C)C>CN(C=O)C.C(#N)C>[O:70]=[C:69]1[NH:65][C@H:66]([C:71]([NH:2][CH:3]2[N:9]=[C:8]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)[C:7]3[CH:16]=[CH:17][CH:18]=[CH:19][C:6]=3[NH:5][C:4]2=[O:20])=[O:72])[CH2:67][CH2:68]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

11

Reactant 8

HCID 111,2-DichloroethaneHCID 7405L-Pyroglutamic AcidHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 180504Ceric ammonium nitrateHCID 6100505Dipotassium 2,3-dihydroxybutanedioate
HCID 18917698
3-amino-2,3-dihydro-2-oxo-5-phenyl-1H-1,4-benzodiazepine hydrogen bromide
HCID 21893785Acetic Acid Mixture with Hydrobromic Acid

Product 1

HCID 229405853-[5-Oxo-pyrrolidine-2(S)-carbonylamino]-2,3-dihydro-2-oxo-5-phenyl-1H-1,4-benzodiazepine

Reagents, catalysts & solvents 2

HCID 6228DimethylformamideSolventHCID 6342AcetonitrileSolvent

Procedure

A solution of 3-amino-2,3-dihydro-2-oxo-5-phenyl-1H-1,4-benzodiazepine hydrogen bromide (142 mg, 0.426 mmol), prepared by sequential treatment of an aqueous acetonitrile solution of the 4-methoxybenzyl derivative from example 5 with ammonium cerium IV nitrate, potassium tartrate solution and HBr/acetic acid--(L)-pyroglutamic acid (60.2 mg, 0.466 mmol), EDC (91 mg, 0.473 mmol), HOBT (63.5 mg, 0.473 mmol), and diisopropylethylamine (0.082 ml, 0.473 mmol) in DMF (5 ml) was stirred at room temperature for 18 hours. The resultant solution was concentrated in vacuo, and the residue partitioned between ethyl acetate and aqueous sodium bicarbonate solution. The organic extract was washed with brine, dried, (MgSO4), filtered, and concentrated. The residue was purified by preparative HPLC (C18, eluted with a 5:95 to 40:60 water:acetonitrile). Lyophilization provided the titled compound as a 1:1 mixture of diastereomers.

Workup

  1. concentrationThe resultant solution was concentrated in vacuo
  2. customthe residue partitioned between ethyl acetate and aqueous sodium bicarbonate solution
  3. extractionThe organic extract
  4. washwas washed with brine
  5. dry with materialdried, (MgSO4),
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe residue was purified by preparative HPLC (C18
  9. washeluted with a 5:95 to 40:60 water

Sources & evidence

ORD record
ord-ea3ed4ab1cee468d83019842b15b5f32
Source dataset
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05852010

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes