Diisopropylethylamine → HCID 86751128, Verbindung

HRID 1939214Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1939214
[S:1]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][NH:5][C:4]=2[CH:3]=[CH:2]1.C(N(CC)C(C)C)(C)C.[N:20]1[CH:25]=[CH:24][CH:23]=[C:22]([C:26]2[S:27][CH:28]=[C:29]([C:31](Cl)=[O:32])[N:30]=2)[CH:21]=1>ClCCl.O>[N:20]1[CH:25]=[CH:24][CH:23]=[C:22]([C:26]2[S:27][CH:28]=[C:29]([C:31]([C:2]3[S:1][C:10]4[CH2:9][CH2:8][CH2:7][CH2:6][NH:5][C:4]=4[CH:3]=3)=[O:32])[N:30]=2)[CH:21]=1

Komponenten

6

Edukt 3

HCID 81531DiisopropylethylamineHCID 118049715,6,7,8-Tetrahydro-4H-thieno[3,2-B]azepineHCID 229945454-Thiazolecarbonyl chloride, 2-(3-pyridinyl)-

Produkt 1

HCID 86751128HCID 86751128, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a cooled (0° C.) solution of 2 mmol of 5,6,7,8-tetrahydro-4H-thieno[3,2-b]azepine, 6 mmol of N,N-diisopropylethylamine in 8 ml of dichloromethane added 2.2 mmol of 2-(3-pyridinyl)thiazole-4-carbonyl chloride. The mixture is stirred at room temperature for 16 hours and diluted with 50 ml of dichloromethane and 25 ml of water. The organic layer is separated, washed with H2O, 1N NaHCO3, brine and dried (Na2SO4). The solvent is removed under vacuum and the residue chromatographed on silica gel with ethyl acetate-hexane as solvent to give the product as a solid.

Aufarbeitung

  1. customThe organic layer is separated
  2. washwashed with H2O, 1N NaHCO3, brine
  3. dry with materialdried (Na2SO4)
  4. customThe solvent is removed under vacuum
  5. customthe residue chromatographed on silica gel with ethyl acetate-hexane as solvent

Quellen und Nachweise

ORD-Eintrag
ord-ffc8f08ac5d94c06858cb726f0be69ec
Quelldatensatz
uspto-grants-1997_12
Patentnummer
US05696112

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