Hydrochloric Acid → HCID 68600205, Verbindung

HRID 1943186Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1943186
[O:1]=[C:2]1[CH:12]=[N:11][C:10]2=[C:13]3[N:3]1[CH2:4][C@@H:5]([CH2:15][N:16]1[CH2:21][CH2:20][CH:19]([NH:22]C(=O)OC(C)(C)C)[CH2:18][CH2:17]1)[N:6]3[C:7](=[O:14])[CH:8]=[CH:9]2.[ClH:30]>C(Cl)(Cl)Cl.O1CCOCC1>[ClH:30].[ClH:30].[NH2:22][CH:19]1[CH2:20][CH2:21][N:16]([CH2:15][C@H:5]2[N:6]3[C:13]4[N:3]([C:2](=[O:1])[CH:12]=[N:11][C:10]=4[CH:9]=[CH:8][C:7]3=[O:14])[CH2:4]2)[CH2:17][CH2:18]1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 866368431,1-Dimethylethyl (1-{[(1R)-3,8-dioxo-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylen-1-yl]methyl}-4-piperidinyl)carbamate

Produkt 1

HCID 68600205HCID 68600205, VerbindungAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A solution of 1,1-dimethylethyl (1-{[(1R)-3,8-dioxo-1,2-dihydro-3H,8H-2a,5,8a-triazaacenaphthylen-1-yl]methyl}-4-piperidinyl)carbamate (76 mg, 0.189 mmol) in chloroform (2 ml) at room temperature was treated with 4M HCl in 1,4-dioxane (2 ml). A solid precipitated out and the mixture was stirred room temperature. After 0.5 h the reaction was complete so some methanol was added to dissolve most of the solid, followed by toluene and all the solvents were removed to afford the product as a dark yellow solid (70.9 mg, 99%).

Aufarbeitung

  1. customA solid precipitated out
  2. additionwas added
  3. dissolutionto dissolve most of the solid
  4. customwere removed

Quellen und Nachweise

ORD-Eintrag
ord-68fc5d47d9a045ed90677d0708d48d26
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08389524B2

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