HCID 18448528, Verbindung → HCID 69431308, Verbindung

HRID 1269464Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1269464
[N:1]1([CH2:7][C:8]([C:10]2[CH:11]=[C:12]3[C:17](=[CH:18][CH:19]=2)[CH:16]([NH:20][C:21](=[O:42])[CH2:22][CH:23]2[CH2:28][CH2:27][CH2:26][CH2:25][N:24]2[S:29]([C:32]2[CH:37]=[CH:36][CH:35]=[C:34]([C:38]([F:41])([F:40])[F:39])[CH:33]=2)(=[O:31])=[O:30])[CH2:15][CH2:14][CH2:13]3)=[CH2:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1>CCO>[CH3:9][C@@H:8]([C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][CH:19]=1)[C@H:16]([NH:20][C:21](=[O:42])[CH2:22][C@@H:23]1[CH2:28][CH2:27][CH2:26][CH2:25][N:24]1[S:29]([C:32]1[CH:37]=[CH:36][CH:35]=[C:34]([C:38]([F:40])([F:41])[F:39])[CH:33]=1)(=[O:31])=[O:30])[CH2:15][CH2:14][CH2:13]2)[CH2:7][N:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Komponenten

3

Edukt 1

HCID 18448528HCID 18448528, Verbindung

Produkt 1

HCID 69431308HCID 69431308, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of N-[6-(1-piperidin-1-ylmethyl-vinyl)-1,2,3,4-tetrahydro-naphthalen-1-yl]-2-[1-(3-trifluoromethyl-benzenesulfonyl)-piperidin-2-yl]-acetamide (34 mg, 0.05 mmol), EtOH (2 mL), Pd/Al2O3 (Johnson Matthey, 12 mg, 0.1 eq) was purged with H2 and connected to a H2 balloon for 30 min at RT. The catalyst was filtered through Celite and washed with MeOH. The filtrate was concentrated in vacuo. The crude was purified by silica gel chromatography (7%–10% MeOH—CH2Cl2) to afford the title compound as a mixture of two diastereomers. MS (ESI): 606 (M+H)+. Calc'd for C32H42F3N3O3S—605.29.

Aufarbeitung

  1. customwas purged with H2
  2. filtrationThe catalyst was filtered through Celite
  3. washwashed with MeOH
  4. concentrationThe filtrate was concentrated in vacuo
  5. customThe crude was purified by silica gel chromatography (7%–10% MeOH—CH2Cl2)

Quellen und Nachweise

ORD-Eintrag
ord-c17da065b3424feb896129c29e10fce1
Quelldatensatz
uspto-grants-2007_04
Patentnummer
US07199244B2

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