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Hydrochloric Acid → M-58996

HRID 1727097
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1727097
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][C:14]([CH2:18][N:19]([CH3:29])[C:20]3[CH:28]=[CH:27][C:23]([C:24]([OH:26])=[O:25])=[CH:22][CH:21]=3)([OH:17])[CH2:13][CH2:12]2)=[CH:5][CH:4]=1)#[N:2].[ClH:30]>C(O)C.O>[ClH:30].[C:1]([C:3]1[CH:4]=[CH:5][C:6]([CH2:9][CH2:10][N:11]2[CH2:12][CH2:13][C:14]([CH2:18][N:19]([CH3:29])[C:20]3[CH:21]=[CH:22][C:23]([C:24]([OH:26])=[O:25])=[CH:27][CH:28]=3)([OH:17])[CH2:15][CH2:16]2)=[CH:7][CH:8]=1)#[N:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 12986481UP9V9DB2RD

Produkt 1

HCID 67371796M-58996

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

The compound (22.0 g) obtained in Example 1 was suspended in a mixture of ethanol (264 mL) and water (176 mL). The mixture was heated under reflux and was completely dissolved by adding 1 N hydrochloric acid (58.7 mL) dropwise while keeping the mixture under reflux. After cooling to room temperature, the precipitated crystals were collected by filtration. The crystals were sequentially washed with 2-propanol (50 mL×3) and tert-butyl methyl ether (50 mL×3), dried under reduced pressure to yield the titled compound (21.1 g) as crystals. Elementary analysis revealed that the compound is monohydrate.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux
  3. dissolutionwas completely dissolved
  4. temperatureunder reflux
  5. filtrationthe precipitated crystals were collected by filtration
  6. washThe crystals were sequentially washed with 2-propanol (50 mL×3) and tert-butyl methyl ether (50 mL×3)
  7. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6c2ab4fadb4c4ac4bd8a415063364d41
Quelldatensatz
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07494987B2

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