Hydrochloric Acid → NPSP795

HRID 2215279Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2215279
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][C:11]([OH:13])=[O:12])=[CH:5][C:4]=1[O:14][CH2:15][C@H:16]([OH:32])[CH2:17][NH:18][C:19]([CH3:31])([CH3:30])[CH2:20][CH:21]1[CH2:29][C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH2:22]1)#[N:2].[ClH:33]>C(#N)C.CCOCC>[ClH:33].[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][C:11]([OH:13])=[O:12])=[CH:5][C:4]=1[O:14][CH2:15][C@H:16]([OH:32])[CH2:17][NH:18][C:19]([CH3:30])([CH3:31])[CH2:20][CH:21]1[CH2:22][C:23]2[C:28](=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH2:29]1)#[N:2]

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 9910902SB-423562

Produkt 1

HCID 68607251NPSP795Ausbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

The compound from Example 4 (80 mg, 0.18 mmol) was suspended in acetonitrile (8 mL) and treated with 1 N hydrogen chloride in ether dropwise with stirring until the solid dissolved. The mixture was quickly filtered and cooled in an ice bath. The white crystalline solid which formed was isolated by filtration, washed with ether, and dried in vacuo to afford the title compound (80 mg, 94%). Mp 180–181° C.; MS(ES) m/e 437.2 [M+H]+.

Aufarbeitung

  1. dissolutiondissolved
  2. filtrationThe mixture was quickly filtered
  3. temperaturecooled in an ice bath
  4. customThe white crystalline solid which formed
  5. customwas isolated by filtration
  6. washwashed with ether
  7. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-3564b0f2d4104ec38ab58cd32ac4b9a4
Quelldatensatz
uspto-grants-2006_09
Patentnummer
US07109238B2

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