Triethylamine → HCID 11675083, Verbindung

HRID 631875Notizen

Reaktionsgleichung

C(=O)([O-])[O-].[Cs+].[Cs+].C(N(CC)CC)C.[CH3:14][O:15][C:16]([C:18]1[C:27]2[CH2:26][CH2:25][CH2:24][CH2:23][C:22]=2[CH:21]=[CH:20][C:19]=1OS(C(F)(F)F)(=O)=O)=[O:17].[C:36](=[NH:49])([C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1>O1CCOCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2>[CH3:14][O:15][C:16]([C:18]1[C:27]2[CH2:26][CH2:25][CH2:24][CH2:23][C:22]=2[CH:21]=[CH:20][C:19]=1[N:49]=[C:36]([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)=[O:17]

Komponenten

Reaktionsbedingungen

Temperatur: 100 °C

Versuchsvorschrift

Cesium carbonate (12.4 g), palladium (II) acetate (0.12 g), triethylamine (0.12 mL) and Xantphos (0.474 g) were suspended in dioxane (50 mL) under nitrogen. 2-Trifluoromethanesulfonyloxy-5,6,7,8-tetrahydronaphthalene-1-carboxylic acid methyl ester (Intermediate 7, 4.2 g) and benzhydrylidenamine (5.5 mL) in dioxane (35 mL) were added and the mixture was heated at 100° C. for 3.5 hours. The resulting mixture was partitioned between ethyl acetate and water. The organic solution was washed with water and concentrated under vacuum. The residue was recrystallised from methanol to give the title compound as an off-white solid (8.2 g).

Aufarbeitung

customThe resulting mixture was partitioned between ethyl acetate and water
washThe organic solution was washed with water
concentrationconcentrated under vacuum
customThe residue was recrystallised from methanol

Quellen und Nachweise

ORD-Eintrag: ord-cd225b3c05224c1d9d141cb68ba8ffbe
Quelldatensatz: uspto-grants-2016_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09321740B2

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