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1,2-Dichloroethane → [2-(3-butoxy-3-o-tolyl-azetidin-1-yl)-1-(4-hydroxybenzyl)-2-oxoethyl]-3-(3H-imidazol-4-yl)propionamide

HRID 540419
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Reaktionsgleichung

Reaktionsgleichung von HRID 540419
[CH2:1](Cl)[CH2:2]Cl.C1C=CC2N(O)N=[N:11]C=2C=1.C(OC(N[C@H:23]([CH2:27][C:28]1[CH:33]=[CH:32][C:31]([OH:34])=[CH:30][CH:29]=1)[C:24]([OH:26])=O)=O)(C)(C)C.FC(F)(F)C(O)=O.[CH2:42]([O:46][C:47]1([C:51]2[CH:56]=[CH:55][CH:54]=[CH:53][C:52]=2[CH3:57])[CH2:50][NH:49][CH2:48]1)[CH2:43][CH2:44][CH3:45].C([N:60]([CH2:63]C)[CH2:61][CH3:62])C.Cl.C[N:67](C)[CH:68]=[O:69]>>[CH2:42]([O:46][C:47]1([C:51]2[CH:56]=[CH:55][CH:54]=[CH:53][C:52]=2[CH3:57])[CH2:48][N:49]([C:24](=[O:26])[CH:23]([CH:1]([CH2:2][C:62]2[NH:11][CH:63]=[N:60][CH:61]=2)[C:68]([NH2:67])=[O:69])[CH2:27][C:28]2[CH:29]=[CH:30][C:31]([OH:34])=[CH:32][CH:33]=2)[CH2:50]1)[CH2:43][CH2:44][CH3:45]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 7

HCID 111,2-DichloroethaneHCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 1549481(2R)-2-(((tert-butoxy)carbonyl)amino)-3-(4-hydroxyphenyl)propanoic acid
HCID 66988065
3-Butoxy-3-o-tolylazetidine trifluoroacetate

Produkt 1

HCID 66988077[2-(3-butoxy-3-o-tolyl-azetidin-1-yl)-1-(4-hydroxybenzyl)-2-oxoethyl]-3-(3H-imidazol-4-yl)propionamideAusbeute 90 %

Versuchsvorschrift

205 mg (1.1 mmol) of EDC and then 145 mg (1.1 mmol) of HOBt are added to a solution of 250 mg (0.9 mmol) of (R)-2-tert-butoxycarbonylamino-3-(4-hydroxyphenyl)-propanoic acid in 5 ml of dimethylformamide. After stirring for 15 minutes at ambient temperature, 300 mg (1.1 mmol) of 3-butoxy-3-o-tolylazetidine trifluoro-acetate (described in Example 15.5) and 0.5 ml (3.6 mmol) of triethylamine are added. The reaction medium is stirred for 2 h at ambient temperature and then a 1N aqueous solution of hydrochloric acid is added and the mixture is extracted with ethyl acetate. The organic phase is washed with water, and then dried over magnesium sulphate, filtered and evaporated. The residue is purified by silica gel chromatography, elution being carried out with a 60/40 heptane/ethyl acetate mixture. 410 mg of [2-(3-butoxy-3-o-tolyl-azetidin-1-yl)-1-(4-hydroxybenzyl)-2-oxoethyl]-3-(3H-imidazol-4-yl)propionamide are obtained with a yield of 90%.

Aufarbeitung

  1. stirringThe reaction medium is stirred for 2 h at ambient temperature
  2. extractionthe mixture is extracted with ethyl acetate
  3. washThe organic phase is washed with water
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is purified by silica gel chromatography, elution

Quellen und Nachweise

ORD-Eintrag
ord-7b3897ad785c40c2aa417f05a9557aaa
Quelldatensatz
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08871187B2

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