Hydrochloric Acid → HCID 131720060, Verbindung

HRID 1066676Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1066676
[F:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:28][CH2:29]OS(C)(=O)=O)[O:14][CH2:13][CH2:12][N:11]([C:15](=[O:27])[CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([O:23][CH:24]([CH3:26])[CH3:25])[CH:18]=3)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].[N:35]1([CH:41]2[CH2:46][CH2:45][NH:44][CH2:43][CH2:42]2)[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]1.O.[ClH:48]>CN(C=O)C.CCOCC>[OH2:14].[ClH:48].[ClH:48].[F:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:28][CH2:29][N:44]3[CH2:45][CH2:46][CH:41]([N:35]4[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]4)[CH2:42][CH2:43]3)[O:14][CH2:13][CH2:12][N:11]([C:15](=[O:27])[CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([O:23][CH:24]([CH3:26])[CH3:25])[CH:18]=3)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].[F:1][C:2]1[CH:3]=[C:4]([C:9]2([CH2:28][CH2:29][N:44]3[CH2:45][CH2:46][CH:41]([N:35]4[CH2:40][CH2:39][CH2:38][CH2:37][CH2:36]4)[CH2:42][CH2:43]3)[O:14][CH2:13][CH2:12][N:11]([C:15](=[O:27])[CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([O:23][CH:24]([CH3:26])[CH3:25])[CH:18]=3)[CH2:10]2)[CH:5]=[CH:6][C:7]=1[F:8].[ClH:48].[ClH:48]

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 786071,4'-BipiperidineHCID 21200564HCID 21200564, Verbindung

Produkt 1

HCID 131720060HCID 131720060, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A mixture of 1.3 g of the compound obtained in step C of EXAMPLE 71 and 1.1 g of 4-(piperid-1-yl)piperidine in 4 ml of DMF is heated at 70° C. for 4 hours. After cooling to RT, the reaction mixture is poured into iced water and extracted with AcOEt, the organic phase is washed with 1 N NaOH solution and with saturated NaCl solution and dried over Na2SO4 and the solvent is evaporated off under vacuum. The residue is chromoatographed on silica H using DCM and then a DCM/MeOH mixture (90/10; v/v) as the eluent. The product obtained is taken up with a saturated solution of hydrochloric acid in ether and the precipitate formed is wrung to give 0.49 g of the expected product. M.p.=270° C. (dec.).

Aufarbeitung

  1. temperatureAfter cooling to RT
  2. extractionextracted with AcOEt
  3. washthe organic phase is washed with 1 N NaOH solution and with saturated NaCl solution
  4. dry with materialdried over Na2SO4
  5. customthe solvent is evaporated off under vacuum
  6. customThe product obtained
  7. customthe precipitate formed

Quellen und Nachweise

ORD-Eintrag
ord-b19b29085b87478092c2a8d294a4c4ec
Quelldatensatz
uspto-grants-2001_06
Patentnummer
US06242637B1

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