4-Methylmorpholine → HCID 178450256, Verbindung

HRID 2365512Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2365512
[CH2:1]([O:5][CH:6]1[CH2:11][CH2:10][N:9]([S:12]([C:15]2[CH:16]=[C:17]([CH:21]=[CH:22][CH:23]=2)[C:18]([OH:20])=O)(=[O:14])=[O:13])[CH2:8][CH2:7]1)[CH:2]([CH3:4])[CH3:3].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.Cl.Cl.[NH:50]1[C:54]2([CH2:59][CH2:58][NH:57][CH2:56][CH2:55]2)[CH2:53][NH:52]/[C:51]/1=[N:60]\[C:61]([C:63]1[C:68]([NH2:69])=[N:67][C:66]([NH2:70])=[C:65]([Cl:71])[N:64]=1)=[O:62].CN1CCOCC1>CN(C=O)C>[CH2:1]([O:5][CH:6]1[CH2:11][CH2:10][N:9]([S:12]([C:15]2[CH:16]=[C:17]([CH:21]=[CH:22][CH:23]=2)[C:18]([N:57]2[CH2:58][CH2:59][C:54]3([NH:50]/[C:51](=[N:60]/[C:61]([C:63]4[C:68]([NH2:69])=[N:67][C:66]([NH2:70])=[C:65]([Cl:71])[N:64]=4)=[O:62])/[NH:52][CH2:53]3)[CH2:55][CH2:56]2)=[O:20])(=[O:14])=[O:13])[CH2:8][CH2:7]1)[CH:2]([CH3:4])[CH3:3]

Komponenten

6

Edukt 4

HCID 79724-MethylmorpholineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 670866863-(4-Isobutoxy-piperidine-1-sulfonyl)-benzoic acidHCID 178478673HCID 178478673, Verbindung

Produkt 1

HCID 178450256HCID 178450256, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

3-(4-Isobutoxy-piperidine-1-sulfonyl)-benzoic acid (0.03 mmol, 10.2 mg) is treated with a solution of HATU (11.4 mg, 0.03 mmol) in DMF (1 ml) followed by a solution of 3,5-Diamino-6-chloro-pyrazine-2-carboxylic acid [1,3,8-triaza-spiro[4.5]dec-(2E)-ylidene]-amide dihydrochloride (Ex. 38) (11.9 mg, 0.03 mmol) and N-methyl morpholine (0.010 ml, 0.03 mmol) in DMF (1 ml) and shaken at room temperature overnight. The solution is evaporated under vacuum, redissolved in DMSO (0.5 ml) and purified by mass-directed preparative HPLC. The purified fractions are evaporated under vacuum to afford the title compound; [M+H]+ 648.4

Aufarbeitung

  1. customThe solution is evaporated under vacuum
  2. dissolutionredissolved in DMSO (0.5 ml)
  3. custompurified by mass-directed preparative HPLC
  4. customThe purified fractions are evaporated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-f90ca3a83890485cb9600e2c52826faf
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08697687B2

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