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Acetic Acid → HCID 178474963, compound

HRID 331403
Notes
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Reaction equation

HRID 331403 reaction equation
Cl.Cl.[O:3]1[C:8]2=[CH:9][CH:10]=[CH:11][C:7]2=[C:6]([CH:12]2[CH2:17][CH2:16][CH2:15][CH2:14][N:13]2[CH2:18][CH2:19][C@H:20]2[CH2:25][CH2:24][C@H:23]([NH2:26])[CH2:22][CH2:21]2)[CH:5]=[CH:4]1.C(N(CC)C(C)C)(C)C.[C:36](O)(=[O:38])[CH3:37].CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.[OH-].[Na+]>CN(C=O)C>[O:3]1[C:8]2=[CH:9][CH:10]=[CH:11][C:7]2=[C:6]([CH:12]2[CH2:17][CH2:16][CH2:15][CH2:14][N:13]2[CH2:18][CH2:19][C@H:20]2[CH2:21][CH2:22][C@H:23]([NH:26][C:36](=[O:38])[CH3:37])[CH2:24][CH2:25]2)[CH:5]=[CH:4]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 178478712HCID 178478712, compound2×

Product 1

HCID 178474963
HCID 178474963, compound
Yield 80.3%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

To a stirred mixture of trans-4-[2-(4-benzofuran-4-yl-piperidin-1-yl)-ethyl]-cyclohexyl-amine dihydrochloride (intermediate A) (100 mg, 0.25 mmol) in DMF (3 ml) was added N,N-diisopropylethylamine (113 mg, 150 μl, 0.88 mmol), acetic acid (22.6 mg, 21.5 μl, 376 μmol) and TBTU (121 mg, 376 μmol). The mixture was allowed to stir at room temperature for 5 h, poured into ice/water (5 ml) and 1N NaOH (5 ml) and extracted with dichloromethane (2×20 ml). The combined organic layers were washed with brine (10 ml), dried (MgSO4) and evaporated. The crude material was further purified by flash chromatography on silica gel (dichloromethane/MeOH/NH4OH 150:10:1) and trituration from dichloromethane (1 ml) and heptane (5 ml) for 30 min. The precipitate was collected by filtration, washed with heptane and dried to yield the title compound as an off-white solid (74 mg, 80%), MS (ISP) m/z=369.3 [(M+H)+], mp 167° C.

Workup

  1. extractionextracted with dichloromethane (2×20 ml)
  2. washThe combined organic layers were washed with brine (10 ml)
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customThe crude material was further purified by flash chromatography on silica gel (dichloromethane/MeOH/NH4OH 150:10:1) and trituration from dichloromethane (1 ml) and heptane (5 ml) for 30 min
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with heptane
  8. customdried

Sources & evidence

ORD record
ord-aceff7a2215949e686238336b18c15c5
Source dataset
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08877778B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes