p-Toluenesulfonic acid monohydrate → HCID 178485563, Verbindung

HRID 334149Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 334149
[CH3:1][NH:2][C:3]([C:5]1[N:6](C2CCCCO2)[C:7]2[C:12]([N:13]=1)=[C:11]([N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)[N:10]=[C:9]([Cl:20])[N:8]=2)=[O:4].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CO.O.C(=O)(O)[O-].[Na+]>[CH3:1][NH:2][C:3]([C:5]1[NH:6][C:7]2[C:12]([N:13]=1)=[C:11]([N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)[N:10]=[C:9]([Cl:20])[N:8]=2)=[O:4]

Komponenten

6

Edukt 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 86667366HCID 86667366, Verbindung

Produkt 1

HCID 178485563HCID 178485563, VerbindungAusbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 516892Sodium BicarbonateLösungsmittel

Versuchsvorschrift

2-Chloro-6-morpholin-4-yl-9-(tetrahydro-pyran-2-yl)-9H-purine-8-carboxylic acid methylamide (104 mg, 0.27 mmol) was suspended in methanol (6 mL) and p-toluenesulfonic acid monohydrate (10 mg, 0.05 mmol) was added. The mixture was stirred at room temperature for 68 h, then diluted with water and neutralized with aqueous sodium bicarbonate. The solid precipitate was filtered off and dried at 50° C. under vacuum to give 2-chloro-6-morpholin-4-yl-9H-purine-8-carboxylic acid methylamide (56 mg, 70%). LCMS RT=2.43, [M+H]+=297/299

Aufarbeitung

  1. filtrationThe solid precipitate was filtered off
  2. customdried at 50° C. under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-1492cf5858164a5db651a26bd2467990
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08883799B2

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