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Tetrahydrofuran → HCID 178483007, compound

HRID 388140
Notes
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Reaction equation

HRID 388140 reaction equation
Br[C:2]1[CH:3]=[CH:4][C:5]2[N:9]=[C:8]([N:10]([CH3:12])[CH3:11])[N:7](C(OC(C)(C)C)=O)[C:6]=2[CH:20]=1.BrC1C=C[C:25]2[N:29]=[C:28](N(C)C)[NH:27][C:26]=2C=1.C(OC(OC(C)(C)C)=O)([O:36][C:37](C)(C)[CH3:38])=O.C(N(CC)CC)C.C[N:57]([C:59]1[CH:64]=[CH:63][CH:62]=[CH:61][N:60]=1)[CH3:58].[O:65]1CCCC1>>[CH3:12][N:10]([CH3:11])[C:8]1[NH:9][C:5]2[CH:4]=[CH:3][C:2]([C:26]3[N:27]=[C:28]4[N:60]([CH2:61][CH:62]5[CH2:63][CH2:64][O:36][CH2:37][CH2:38]5)[C:59](=[O:65])[NH:57][C:58]4=[N:29][CH:25]=3)=[CH:20][C:6]=2[N:7]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 6

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 218852-DimethylaminopyridineHCID 90495Di-tert-butyl dicarbonateHCID 594745206-Bromo-N,N-dimethyl-1H-benzimidazol-2-amineHCID 66699934HCID 66699934, compound

Product 1

HCID 178483007
HCID 178483007, compound
Yield 54%

Procedure

tert-Butyl 6-bromo-2-(dimethylamino)-1H-benzo[d]imidazole-1-carboxylate. A solution of 6-bromo-N,N-dimethyl-1H-benzo[d]imidazol-2-amine (0.5 g, 2.08 mmol), di-tert-butyl dicarbonate (0.54 g, 2.5 mmol), triethylamine (0.35 mL, 2.55 mmol) and dimethylaminopyridine (few crystals) in anhydrous tetrahydrofuran (10 mL) was allowed to stir at room temperature overnight. The reaction mixture was concentrated under reduced pressure and the crude product was purified by Biotage chromatography (0-55% ethyl acetate in hexanes) to provide the desired product (0.32 g, 54%) as a white solid. MS (ESI) m/z 341.3 [M+1]+.

Workup

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe crude product was purified by Biotage chromatography (0-55% ethyl acetate in hexanes)

Sources & evidence

ORD record
ord-419f85ebb60e4f729c7304ed577cde50
Source dataset
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08372976B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes