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Methanesulfonic Acid → 4-({1-[2-(4-Cyanophenyl)ethyl]-4-hydroxypiperidin-4-ylmethyl}methylamino)benzoic acid monomethanesulfonate

HRID 1727104
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1727104
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[C:6]([C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][C:19]([CH2:23][N:24]([CH3:34])[C:25]3[CH:33]=[CH:32][C:28]([C:29]([OH:31])=[O:30])=[CH:27][CH:26]=3)([OH:22])[CH2:18][CH2:17]2)=[CH:10][CH:9]=1)#[N:7]>O>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[C:6]([C:8]1[CH:9]=[CH:10][C:11]([CH2:14][CH2:15][N:16]2[CH2:17][CH2:18][C:19]([CH2:23][N:24]([CH3:34])[C:25]3[CH:26]=[CH:27][C:28]([C:29]([OH:31])=[O:30])=[CH:32][CH:33]=3)([OH:22])[CH2:20][CH2:21]2)=[CH:12][CH:13]=1)#[N:7]
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Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 12986481UP9V9DB2RD

Produkt 1

HCID 866033484-({1-[2-(4-Cyanophenyl)ethyl]-4-hydroxypiperidin-4-ylmethyl}methylamino)benzoic acid monomethanesulfonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Methanesulfonic acid (1.42 mL) was added to a suspension of the compound (7.2 g) obtained in Example 1 in water (50 mL), was heated with stirring until the compound was dissolved, followed by cooling to room temperature with stirring. The crystals were collected by filtration and were recrystallized from water (50 mL). The resulting crystals were collected by filtration, washed with acetone, and dried under reduced pressure to yield the titled compound (7.6 g) as crystals.

Aufarbeitung

  1. temperaturewas heated
  2. dissolutionwas dissolved
  3. stirringwith stirring
  4. filtrationThe crystals were collected by filtration
  5. customwere recrystallized from water (50 mL)
  6. filtrationThe resulting crystals were collected by filtration
  7. washwashed with acetone
  8. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-5dc419a3ae4b4cd88ac5cdc37ac19b4c
Quelldatensatz
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07494987B2

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