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Triethylamine → 3-(2-Iodo-phenylcarbamoyl)-azetidine-1-carboxylic acid benzyl ester

HRID 528746
Notes
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Reaction equation

HRID 528746 reaction equation
[I:1]NC1C=CC=CC=1.F[P-](F)(F)(F)(F)F.[N:16]1(O[P+](N(C)C)(N(C)C)N(C)C)[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2N=N1.[CH2:36]([O:43][C:44]([N:46]1[CH2:49][CH:48]([C:50]([OH:52])=O)[CH2:47]1)=[O:45])[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1.C(N(CC)CC)C.C([O-])([O-])=O.[Na+].[Na+]>C(#N)C>[CH2:36]([O:43][C:44]([N:46]1[CH2:49][CH:48]([C:50](=[O:52])[NH:16][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[I:1])[CH2:47]1)=[O:45])[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 8471Triethylamine2×HCID 10340Sodium CarbonateHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate2×HCID 109882141-[(Benzyloxy)carbonyl]azetidine-3-carboxylic acidHCID 18447960Iodoaniline

Product 1

HCID 67456254
3-(2-Iodo-phenylcarbamoyl)-azetidine-1-carboxylic acid benzyl ester

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

To 1.0 g (4.57 mmol) iodoaniline in 30 mL acetonitrile were added 2.22 g (5.02 mmol) BOP, 1.78 g (4.57 mmol) azetidine-1,3-dicarboxylic acid monobenzyl ester (route 13, step a), 0.6 mL (4.57 mmol) triethylamine, and the mixture was stirred at room temperature for 16 hours. 0.6 mL (4.57 mmol) triethylamine was added and the mixture was stirred for 2 hours. 2.22 g (5.02 mmol) BOP was added and the mixture was stirred at room temperature for 16 hours. 30 mL 1 M aqueous Na2CO3 was added and the mixture was extracted with EtOAc (2×30 mL), the organic layers were combined, washed with 30 mL brine then dried with Na2SO4. After filtration and evaporation of the solvent the product was purified by column chromatography (silica, heptane/EtOAc 7:3).

Workup

  1. stirringthe mixture was stirred for 2 hours
  2. stirringthe mixture was stirred at room temperature for 16 hours
  3. extractionthe mixture was extracted with EtOAc (2×30 mL)
  4. washwashed with 30 mL brine
  5. dry with materialthen dried with Na2SO4
  6. filtrationAfter filtration and evaporation of the solvent the product
  7. customwas purified by column chromatography (silica, heptane/EtOAc 7:3)

Sources & evidence

ORD record
ord-4d605f15ccd44d6ab539dec074437487
Source dataset
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09346816B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes