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Sodium Hydroxide → tert-butyl (2S)-2-[(4-{[(3,4-dichlorophenyl)amino]-carbonyl}piperazin-1-yl)methyl]morpholine-4-carboxylate

HRID 2371158
Notes
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Reaction equation

HRID 2371158 reaction equation
CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.O[CH2:24][C@@H:25]1[O:30][CH2:29][CH2:28][N:27]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:26]1.S([O-])([O-])(=O)=S.[Na+].[Na+].Cl.[Cl:46][C:47]1[CH:48]=[C:49]([NH:54][C:55]([N:57]2[CH2:62][CH2:61][NH:60][CH2:59][CH2:58]2)=[O:56])[CH:50]=[CH:51][C:52]=1[Cl:53].C(N(CC)C(C)C)(C)C.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].[OH-].[Na+]>C(Cl)Cl>[Cl:46][C:47]1[CH:48]=[C:49]([NH:54][C:55]([N:57]2[CH2:62][CH2:61][N:60]([CH2:24][C@@H:25]3[O:30][CH2:29][CH2:28][N:27]([C:31]([O:33][C:34]([CH3:35])([CH3:36])[CH3:37])=[O:32])[CH2:26]3)[CH2:59][CH2:58]2)=[O:56])[CH:50]=[CH:51][C:52]=1[Cl:53]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

9

Reactant 7

HCID 14798Sodium HydroxideHCID 24477Sodium ThiosulfateHCID 81531DiisopropylethylamineHCID 159087TriacetoxyperiodinaneHCID 1512576(R)-N-Boc-2-hydroxymethylmorpholineHCID 5049666Sodium triacetoxyborohydride
HCID 46743200
N-(3,4-dichlorophenyl)piperazine-1-carboxamide hydrochloride

Product 1

HCID 57656853tert-butyl (2S)-2-[(4-{[(3,4-dichlorophenyl)amino]-carbonyl}piperazin-1-yl)methyl]morpholine-4-carboxylateYield 24.1%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

Dess-Martin periodinane (8.60 g) was added to tert-butyl (2R)-2-(hydroxymethyl)morpholine-4-carboxylate (4.00 g) in dry DCM at 0° C. The reaction was warmed to RT and stirred for a further 2 h. Aqueous sodium thiosulfate (10% w/v, 50 ml) was added and the DCM layer was removed then dried (MgSO4), filtered and evaporated to form the crude aldehyde. The residue was then dissolved in dry dichloromethane (100 ml) followed by addition of N-(3,4-dichlorophenyl)piperazine-1-carboxamide hydrochloride (5.72 g), N, N-diisopropylethylamine (3.17 mL) and NaBH(OAc)3 (9.76 g) and the reaction was stirred under argon for 18 h. 1M NaOH (50 mL) was added followed by vigorous stirring and the dichloromethane layer was extracted. The organic layer was dried (MgSO4), filtered and evaporated. Purification by chromatography (EtOAc neat) afforded the title compound (2.10 g) as a white foam.

Workup

  1. customthe DCM layer was removed
  2. dry with materialthen dried (MgSO4)
  3. filtrationfiltered
  4. customevaporated
  5. customto form the crude aldehyde
  6. stirringthe reaction was stirred under argon for 18 h
  7. stirringby vigorous stirring
  8. extractionthe dichloromethane layer was extracted
  9. dry with materialThe organic layer was dried (MgSO4)
  10. filtrationfiltered
  11. customevaporated
  12. customPurification by chromatography (EtOAc neat)

Sources & evidence

ORD record
ord-0528fbe1ee724e589af00e0ed62e119d
Source dataset
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08710224B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes