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Phosphorus pentachloride → 5-Isopropyl-pyridine-2-sulphonic acid 5-(2-chloro-5-methoxy-phenoxy)-6-chloromethyl-2-morpholin-4-yl-pyrimidin-4-ylamide

HRID 356654
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 356654
[Cl:1][C:2]1[CH:35]=[CH:34][C:33]([O:36][CH3:37])=[CH:32][C:3]=1[O:4][C:5]1[C:6]([NH:19][S:20]([C:23]2[CH:28]=[CH:27][C:26]([CH:29]([CH3:31])[CH3:30])=[CH:25][N:24]=2)(=[O:22])=[O:21])=[N:7][C:8]([N:13]2[CH2:18][CH2:17][O:16][CH2:15][CH2:14]2)=[N:9][C:10]=1[CH2:11]O.P(Cl)(Cl)(Cl)(Cl)[Cl:39]>O=P(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:35]=[CH:34][C:33]([O:36][CH3:37])=[CH:32][C:3]=1[O:4][C:5]1[C:6]([NH:19][S:20]([C:23]2[CH:28]=[CH:27][C:26]([CH:29]([CH3:31])[CH3:30])=[CH:25][N:24]=2)(=[O:22])=[O:21])=[N:7][C:8]([N:13]2[CH2:14][CH2:15][O:16][CH2:17][CH2:18]2)=[N:9][C:10]=1[CH2:11][Cl:39]
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Komponenten

4

Edukt 2

HCID 24819Phosphorus pentachlorideHCID 178683755-Isopropyl-pyridine-2-sulphonic acid 5-(2-chloro-5-methoxy-phenoxy)-6-hydroxymethyl-2-morpholin-4-yl-pyrimidin-4-ylamide

Produkt 1

HCID 223778495-Isopropyl-pyridine-2-sulphonic acid 5-(2-chloro-5-methoxy-phenoxy)-6-chloromethyl-2-morpholin-4-yl-pyrimidin-4-ylamideAusbeute 72,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24813
Phosphorus oxychloride
Lösungsmittel

Versuchsvorschrift

0.2 g of the compound obtained in Example 38 in 3.5 ml of POCl3 was stirred with 0.083 g of PCl5 at 20° C. for 2 hours. Thereafter, the POCl3 was distilled off and the residue was partitioned between ethyl acetate and aqueous sodium bicarbonate (sic). The organic phase was washed with water, dried and the solvent was evaporated. The residue was chromatographed over silica gel with chloroform-methanol, thereafter recrystallized from dichloromethane-ethanol. 0.150 g of 5-isopropyl-pyridine-2-sulphonic acid 5-(2-chloro-5-methoxy-phenoxy)-6-chloromethyl-2-morpholin-4-yl-pyrimidin-4-ylamide, m.p. 205° C., was obtained.

Aufarbeitung

  1. distillationThereafter, the POCl3 was distilled off
  2. customthe residue was partitioned between ethyl acetate and aqueous sodium bicarbonate (sic)
  3. washThe organic phase was washed with water
  4. customdried
  5. customthe solvent was evaporated
  6. customThe residue was chromatographed over silica gel with chloroform-methanol
  7. customrecrystallized from dichloromethane-ethanol

Quellen und Nachweise

ORD-Eintrag
ord-ae53e6594c4747139f01ab4a54ad25bf
Quelldatensatz
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05837708

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