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Phosgene → WAY127093B racemate

HRID 1612945
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1612945
[C:1](Cl)(Cl)=[O:2].C(N(CC)CC)C.[N:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][NH2:19])[CH:13]=1.[CH:20]1([O:25][C:26]2[CH:27]=[C:28]([CH:34]3[N:38]([CH3:39])[NH:37][C:36](=[O:40])[CH2:35]3)[CH:29]=[CH:30][C:31]=2[O:32][CH3:33])[CH2:24][CH2:23][CH2:22][CH2:21]1>O1CCCC1>[CH:20]1([O:25][C:26]2[CH:27]=[C:28]([CH:34]3[CH2:35][C:36](=[O:40])[N:37]([C:1]([NH:19][CH2:18][C:14]4[CH:13]=[N:12][CH:17]=[CH:16][CH:15]=4)=[O:2])[N:38]3[CH3:39])[CH:29]=[CH:30][C:31]=2[O:32][CH3:33])[CH2:21][CH2:22][CH2:23][CH2:24]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 6371PhosgeneHCID 8471Triethylamine2×HCID 310183-PyridinemethanamineHCID 197927655-[3-(Cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone

Produkt 1

HCID 19792796WAY127093B racemate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028
Tetrahydrofuran
Lösungsmittel
3×

Reaktionsbedingungen

Temperatur
-15 °C

Versuchsvorschrift

To a -15° C. solution of phosgene (4.50 mmol, 2.30 mL; 1.9M solution in toluene) in dry tetrahydrofuran (8 mL) is added neat triethylamine (4.50 mmol, 0.450 g; 0.620 mL) and the resulting suspension is stirred at -15° C. for 10 minutes. To this suspension is added 3-picolylamine (4.50 mmol, 0.490 g; 0.460 mL) and triethylamine (4.50 mmol, 0.450 g; 0.620 mL) in dry tetrahydrofuran (10 mL) in one portion and the reaction mixture is stirred at -15° C. for 30 minutes. Subsequently, 5-[3-(cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone (3.0 mmol, 0.870 g) in dry tetrahydrofuran (7 mL) is added at -15° C. and the reaction mixture is allowed to warm to room temperature overnight. The reaction is quenched with water (20 mL), the volatiles removed in vacuo, and the residue partitioned between ethyl acetate (150 mL) and water (150 mL). The organic layer is dried (Na2SO4) and concentrated in vacuo to give a tan solid. This material is purified by flash chromatography (SiO2 :1) 50% ethyl acetate/hexane; 2) 100% ethyl acetate; 3) 5% methanol/ethyl acetate) to give a mixture of starting material and product which is triturated with ether. The title compound is isolated as a white solid (0.158 g; 12%). Also isolated is a mixture of starting pyridazone and title compound (0.511 g). 1H-NMR (DMSO-d6, 400 MHz) δ8.45 (m, 3H); 7.65 (dt, 1H, J=8.0, 1.6 Hz); 7.22 (ddd, 1H, J=8.0, 5.0, 0.7 Hz); 6.94 (d, 1H, J=2.0 Hz); 6.88 (d, 1H, J=8.0 Hz); 6.82 (dd, 1H, J=8.0, 2.0 Hz); 4.63 (m, 1H); 4.38 (m, 3H); 3.70 (s, 3H); 3.65 (m, 1H); 2.74 (s, 3H); 2.65 (m, 1H); 1.79 (m, 2H); 1.63 (m, 4H); 1.49 (m, 2H). IR (KBr, cm-1) 3420, 3320, 2950, 1730, 1715, 1530, 1515, 1235, 1135.

Aufarbeitung

  1. stirringthe reaction mixture is stirred at -15° C. for 30 minutes
  2. temperatureto warm to room temperature overnight
  3. customThe reaction is quenched with water (20 mL)
  4. customthe volatiles removed in vacuo
  5. customthe residue partitioned between ethyl acetate (150 mL) and water (150 mL)
  6. dry with materialThe organic layer is dried (Na2SO4)
  7. concentrationconcentrated in vacuo
  8. customto give a tan solid
  9. customThis material is purified by flash chromatography (SiO2 :1) 50% ethyl acetate/hexane
  10. custom3) 5% methanol/ethyl acetate) to give
  11. additiona mixture of starting material and product which
  12. customis triturated with ether

Quellen und Nachweise

ORD-Eintrag
ord-b2e0ff8677dd47e6bf9d4c5d9b5902ee
Quelldatensatz
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05191084

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