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

HRID 528746
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 528746
[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
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

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

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

  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)

Quellen und Nachweise

ORD-Eintrag
ord-4d605f15ccd44d6ab539dec074437487
Quelldatensatz
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09346816B2

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