Triethylamine → N,O-dimethyl-N-(1-trityl-piperidine-4-carbonyl)hydroxylamine

HRID 278571

Reaktionsgleichung

Reaktionsgleichung von HRID 278571
[C:1]([N:20]1[CH2:25][CH2:24][CH:23]([C:26]([OH:28])=O)[CH2:22][CH2:21]1)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[CH3:30][O:31][NH:32][CH3:33].C(N(CC)CC)C.CCN=C=NCCCN(C)C>ClCCl>[CH3:33][N:32]([O:31][CH3:30])[C:26]([CH:23]1[CH2:22][CH2:21][N:20]([C:1]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH2:25][CH2:24]1)=[O:28]

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 205201821-Tritylpiperidine-4-carboxylic acid

Produkt 1

HCID 22628088N,O-dimethyl-N-(1-trityl-piperidine-4-carbonyl)hydroxylamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a mixture of 1-tritylpiperidine-4-carboxylic acid (7.0 g), O,N-dimethylhydroxylamine hydrochloride (2.0 g) and triethylamine (2.9 ml) in dichloromethane (70 ml) was added WSC (3.97 g), and the mixture was stirred at room temperature for 1 hour and concentrated. To the residue was added ethyl acetate, and the mixture was washed with water, dried (MgSO4) and concentrated. The resulting crystals (6.3 g) were washed with isopropylether.

Aufarbeitung

  1. concentrationconcentrated
  2. additionTo the residue was added ethyl acetate
  3. washthe mixture was washed with water
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. washThe resulting crystals (6.3 g) were washed with isopropylether

Quellen und Nachweise

ORD-Eintrag
ord-13e3f414752049a18edaff60a4782d74
Quelldatensatz
uspto-grants-2002_03
Patentnummer
US06359134B1

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