Hydrochloric Acid → N-(2-t-Butyl-5-{3-[2-(1-imidazolyl)acetoxy]-4-cyclohexylbutyl}phenyl)-2-(9H-xanthen-9-yl)acetamide hydrochloride

HRID 977847Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 977847
O1CCOCC1.[ClH:7].[C:8]([C:12]1[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][CH:20]([O:28][C:29](=[O:36])[CH2:30][N:31]2[CH:35]=[CH:34][N:33]=[CH:32]2)[CH2:21][CH:22]2[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]2)=[CH:14][C:13]=1[NH:37][C:38](=[O:54])[CH2:39][CH:40]1[C:53]2[CH:52]=[CH:51][CH:50]=[CH:49][C:48]=2[O:47][C:46]2[C:41]1=[CH:42][CH:43]=[CH:44][CH:45]=2)([CH3:11])([CH3:10])[CH3:9]>C(OCC)C>[ClH:7].[C:8]([C:12]1[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][CH:20]([O:28][C:29](=[O:36])[CH2:30][N:31]2[CH:35]=[CH:34][N:33]=[CH:32]2)[CH2:21][CH:22]2[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]2)=[CH:14][C:13]=1[NH:37][C:38](=[O:54])[CH2:39][CH:40]1[C:41]2[CH:42]=[CH:43][CH:44]=[CH:45][C:46]=2[O:47][C:48]2[C:53]1=[CH:52][CH:51]=[CH:50][CH:49]=2)([CH3:11])([CH3:9])[CH3:10]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 19966206HCID 19966206, Verbindung

Produkt 1

HCID 19966205N-(2-t-Butyl-5-{3-[2-(1-imidazolyl)acetoxy]-4-cyclohexylbutyl}phenyl)-2-(9H-xanthen-9-yl)acetamide hydrochlorideAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

200 μl of a 4N dioxane solution of hydrogen chloride were added to a solution of 339 mg (0.54 mmol) of N-(2-t-butyl-5-{3-[2-(1-imidazolyl)acetoxy]-4-cyclohexylbutyl}phenyl)-2-(9H-xanthen-9-yl)acetamide [prepared as described in step (i) above] in 3 ml of diethyl ether, and the crystals which precipitated were collected by filtration and washed with diethyl ether. The crystals were purified by high performance liquid chromatography through ODS (120 A, φ30 mm×250 mm) using a 3:1 by volume mixture of acetonitrile and water as the eluent, to give a gel. This gel was crystallized by trituration with diethyl ether, to give 170 mg (yield 85%) of the title compound as colorless crystals, melting at 125°-133° C.

Aufarbeitung

  1. customthe crystals which precipitated
  2. filtrationwere collected by filtration
  3. washwashed with diethyl ether
  4. customThe crystals were purified by high performance liquid chromatography through ODS (120 A, φ30 mm×250 mm)
  5. additionby volume mixture of acetonitrile and water as the eluent
  6. customto give a gel
  7. customThis gel was crystallized by trituration with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-c8dc89b5f2de48b1be2a32b87a266166
Quelldatensatz
uspto-grants-1997_03
Patentnummer
US05614550

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