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Methanesulfonic Acid → 4-Hydroxymethyl-2-meth yl-8-[2'-(1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8-dihydro-6H-pyrido[2,3-d]pyrimidin-7-one

HRID 129015
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 129015
[OH:1][CH2:2][C:3]1[C:4]2[CH2:13][CH2:12][C:11](=[O:14])[N:10]([CH2:15][C:16]3[CH:21]=[CH:20][C:19]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=4[C:28]4[N:32](C(C)(C)C)[N:31]=[N:30][N:29]=4)=[CH:18][CH:17]=3)[C:5]=2[N:6]=[C:7]([CH3:9])[N:8]=1.CS(O)(=O)=O>C1(C)C=CC=CC=1>[OH:1][CH2:2][C:3]1[C:4]2[CH2:13][CH2:12][C:11](=[O:14])[N:10]([CH2:15][C:16]3[CH:17]=[CH:18][C:19]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=4[C:28]4[NH:32][N:31]=[N:30][N:29]=4)=[CH:20][CH:21]=3)[C:5]=2[N:6]=[C:7]([CH3:9])[N:8]=1
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Komponenten

4

Edukt 2

HCID 6395Methanesulfonic AcidHCID 193730024-hydroxymethyl-2-methyl-8-[2'-(1-tert-butyl-1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8-dihydro-6H-pyrido[2,3-d]pyrimidin-7-one

Produkt 1

HCID 1784329704-Hydroxymethyl-2-meth yl-8-[2'-(1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8-dihydro-6H-pyrido[2,3-d]pyrimidin-7-oneAusbeute 19,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140Toluene
Lösungsmittel

Versuchsvorschrift

A mixture of 4-hydroxymethyl-2-methyl-8-[2'-(1-tert-butyl-1H-tetrazol-5-yl)biphenyl-4-ylmethyl]-5,8-dihydro-6H-pyrido[2,3-d]pyrimidin-7-one (550 mg, 1.14 mmol), methanesulfonic acid (1.10 g, 11.40 mmol), and toluene (10 mL) was heated under reflux for 4 days. The mixture was concentrated, 1N KOH (11.4 mL) was added, and the mixture was extracted with CHCl3 (discarded). The aqueous phase was acidified to pH4-5 with 1N HCl and extracted with CHCl3. The extracts were dried and concentrated to give 94 mg of a yellow foam. Trituration with acetone and recrystallization from EtOH gave 46 mg (9%) of product as a white solid, mp 246°-247° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 4 days
  3. concentrationThe mixture was concentrated
  4. addition1N KOH (11.4 mL) was added
  5. extractionthe mixture was extracted with CHCl3 (discarded)
  6. extractionextracted with CHCl3
  7. customThe extracts were dried
  8. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-85207125f9f84de9a5ff1d4f7615041e
Quelldatensatz
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05466692

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