Water → 2-[1-(2-Fluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]pyrazol-3-yl]-5-methoxy pyrimidine-4,6-diamine

HRID 1482926Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1482926
[F:1][C:2]1[CH:19]=[CH:18][CH:17]=[CH:16][C:3]=1[CH2:4][N:5]1[C:9]2[CH2:10][CH2:11][CH2:12][C:8]=2[C:7]([C:13](=[NH:15])[NH2:14])=[N:6]1.[CH3:20][O:21][CH:22]([C:25]#[N:26])[C:23]#[N:24].O>CN(C=O)C>[F:1][C:2]1[CH:19]=[CH:18][CH:17]=[CH:16][C:3]=1[CH2:4][N:5]1[C:9]2[CH2:10][CH2:11][CH2:12][C:8]=2[C:7]([C:13]2[N:14]=[C:25]([NH2:26])[C:22]([O:21][CH3:20])=[C:23]([NH2:24])[N:15]=2)=[N:6]1

Komponenten

5

Edukt 3

HCID 962WaterHCID 108553832-MethoxymalononitrileHCID 866920921-(2-Fluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]pyrazole-3-carboximidamide

Produkt 1

HCID 1180726712-[1-(2-Fluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]pyrazol-3-yl]-5-methoxy pyrimidine-4,6-diamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

100 mg of 1-(2-fluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]pyrazole-3-carboximidamide 1-2-4 (0.39 mmol, 1.0 eq.) and 37 mg methoxymalononitrile (0.39 mmol, 1.0 eq.; for preparation see: US2003/144538 A1, 2003) were dissolved in 1 mL DMF. The mixture was heated for 30 min in a microwave oven at 100° C. After addition of 10 mL water, the precipitated, crude product was filtered off and was purified by flash chromatography yielding 66 mg (0.19 mmol, 48%) of analytically pure target compound.

Aufarbeitung

  1. filtrationthe precipitated, crude product was filtered off
  2. customwas purified by flash chromatography
  3. customyielding 66 mg (0.19 mmol, 48%) of analytically pure target compound

Quellen und Nachweise

ORD-Eintrag
ord-1a1831be05234f02b6b80e9cd5861de9
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09416125B2

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