Triethylamine → HCID 67391050, Verbindung

HRID 906442Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 906442
[N:1]1([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[Br:22][C:23]1[CH:24]=[C:25]2[C:30](=[CH:31][CH:32]=1)[C:29](=[O:33])[NH:28][CH:27]=[C:26]2[S:34](Cl)(=[O:36])=[O:35]>C1COCC1>[Br:22][C:23]1[CH:24]=[C:25]2[C:30](=[CH:31][CH:32]=1)[C:29](=[O:33])[NH:28][CH:27]=[C:26]2[S:34]([N:4]1[CH2:5][CH2:6][CH2:7][N:1]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:2][CH2:3]1)(=[O:36])=[O:35]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 2756058Tert-butyl 1,4-diazepane-1-carboxylateHCID 574399006-Bromo-1-oxo-1,2-dihydroisoquinoline-4-sulfonyl chloride

Produkt 1

HCID 67391050HCID 67391050, VerbindungAusbeute 72,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a solution of tert-butyl 1,4-diazepane-1-carboxylate (0.621 g) and triethylamine (0.864 mL) in THF (12 mL) was added dropwise a solution of 6-bromo-1-oxo-1,2-dihydroisoquinoline-4-sulfonyl chloride (Example 46a, 1 g) in THF (20 mL). The reaction was stirred at room temperature for 20 min. The resulting solution was concentrated under reduced pressure, acidified with 2 M HCl, and extracted into ethyl acetate. The combined organics were dried (MgSO4), filtered and evaporated under reduced pressure to give the subtitle compound (1.097 g) that was used without further purification.

Aufarbeitung

  1. concentrationThe resulting solution was concentrated under reduced pressure
  2. extractionextracted into ethyl acetate
  3. dry with materialThe combined organics were dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d40b05ca164147fabfb0fb1ea4d392dc
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08012980B2

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