Dichloromethane → HCID 20689421, Verbindung
Reaktionsgleichung
[Br:1][C:2]1[CH:21]=[CH:20][C:5]([CH2:6][CH:7]2[CH2:12][CH2:11][N:10](C(OC(C)(C)C)=O)[CH2:9][CH2:8]2)=[CH:4][CH:3]=1.C(Cl)Cl.C(O)(C(F)(F)F)=O>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][CH:7]2[CH2:8][CH2:9][NH:10][CH2:11][CH2:12]2)=[CH:20][CH:21]=1Komponenten
4
Versuchsvorschrift
To a solution of tert-butyl 4-(4-bromobenzyl)piperidine-1-carboxylate (780 mg, 2.2 mmol) in CH2Cl2 (15 mmol), was added TFA (0.5 mL) and the mixture was stirred at rt for 1 h. The solvent was removed in vacuo and the residue dissolved into CH2Cl2 (50 mL), washed with NaOH (0.1 M, 10 mL), brine (10 mL), dried over MgSO4 and concentrated to dryness to give the title compound as a beige solid (520 mg, 93%).
Aufarbeitung
- customThe solvent was removed in vacuo
- dissolutionthe residue dissolved into CH2Cl2 (50 mL)
- washwashed with NaOH (0.1 M, 10 mL), brine (10 mL)
- dry with materialdried over MgSO4
- concentrationconcentrated to dryness
Quellen und Nachweise
- ORD-Eintrag
- ord-77409a7a9ef44bada38ec9add6197bec
- Quelldatensatz
- uspto-grants-2013_07
- Patentnummer
- US08481525B2
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