Hydrochloric Acid → 2-(4-((2-Amino-4-methyl-6-(pentylamino)pyrimidin-5-yl)methyl)phenyl)acetic acid hydrochloride

HRID 445056Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 445056
[NH2:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([CH2:16][C:17]([OH:19])=[O:18])=[CH:12][CH:11]=2)=[C:4]([NH:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[N:3]=1.[ClH:26].C(OC(C)C)(=O)C>C(#N)C>[ClH:26].[NH2:1][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([CH2:9][C:10]2[CH:11]=[CH:12][C:13]([CH2:16][C:17]([OH:19])=[O:18])=[CH:14][CH:15]=2)=[C:4]([NH:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[N:3]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 7915Isopropyl AcetateHCID 595906372-(4-((2-Amino-4-methyl-6-(pentylamino)pyrimidin-5-yl)methyl)phenyl)acetic acid

Produkt 1

HCID 684321402-(4-((2-Amino-4-methyl-6-(pentylamino)pyrimidin-5-yl)methyl)phenyl)acetic acid hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

A suspension of the product from step (v) (8.00 g, 23.4 mmol) in acetonitrile (48.0 g) was heated to 40° C., and 35% aq. HCl (2.68 g, 25.7 mmol) was slowly added to the suspension. After the mixture was stirred at 40° C. for 1 hour, isopropyl acetate (160 g) was slowly added to the mixture. The mixture was cooled to 15° C. and stirred for 1 hour. The resulting precipitate was collected by filtration, washed with combined solution of acetonitrile (5.14 g) and isopropyl acetate (13.9 g), and dried to give the subtitle compound as a white solid, 8.27 g.

Aufarbeitung

  1. temperatureThe mixture was cooled to 15° C.
  2. stirringstirred for 1 hour
  3. filtrationThe resulting precipitate was collected by filtration
  4. washwashed with combined solution of acetonitrile (5.14 g) and isopropyl acetate (13.9 g)
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-15a02acb226f415fa29897ee698a9412
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08476288B2

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