Hydrochloric Acid → HCID 46945559, Verbindung

HRID 2370600Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2370600
Cl.[CH3:2][C:3]1([CH3:49])[C:7](=[O:8])[N:6]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][S:16]([NH:19]C(=O)OC(C)(C)C)(=[O:18])=[O:17])=[C:11]([CH3:27])[CH:10]=2)[C:5](=[O:28])[N:4]1[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][S:38][CH2:39][CH2:40][CH2:41][C:42]([F:48])([F:47])[C:43]([F:46])([F:45])[F:44].C(Cl)Cl.CCOC(C)=O>C(OCC)C>[CH3:2][C:3]1([CH3:49])[C:7](=[O:8])[N:6]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][S:16]([NH2:19])(=[O:18])=[O:17])=[C:11]([CH3:27])[CH:10]=2)[C:5](=[O:28])[N:4]1[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][S:38][CH2:39][CH2:40][CH2:41][C:42]([F:48])([F:47])[C:43]([F:44])([F:45])[F:46]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 21226138Dichloromethane ethylacetateHCID 123569579HCID 123569579, Verbindung

Produkt 1

HCID 46945559HCID 46945559, VerbindungAusbeute 76 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of HCl in ethyl ether (2N, 3 ml) is added in 31-ml portions to a solution of Example 29 (250 mg, 0.36 mmole) in a CH2Cl2/AcOEt mixture (5 ml/3 ml) cooled down to 0° C., and the mixture is stirred for 60 hours at 23° C. The volatiles are evaporated off under vacuum and the residue is taken up in a CH2Cl2 (50 ml) and NaHCO3 (50 ml) mixture. After stirring and decantation, the organic phase is washed with water (50 ml) followed by salt water. After drying over Na2SO4, filtration and concentration to dryness, the residue is purified on a silica column (Heptane/AcOEt:10/0 to 1/1). The expected product is obtained in the form of a white solid with a yield of 76%. Melting point: 102-104° C.

Aufarbeitung

  1. customThe volatiles are evaporated off under vacuum
  2. stirringAfter stirring
  3. washdecantation, the organic phase is washed with water (50 ml)
  4. dry with materialAfter drying over Na2SO4, filtration and concentration to dryness
  5. customthe residue is purified on a silica column (Heptane/AcOEt:10/0 to 1/1)

Quellen und Nachweise

ORD-Eintrag
ord-77e5e8f591b04f6985924204104dd802
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08710091B2

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