Hydrogen chloride-ethyl acetate → Benzyl benzyl[cis(+/-)-3-methoxypiperidin-4-yl]carbamate

HRID 1425439Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1425439
Cl.C(OCC)(=O)C.[CH2:8]([N:15]([C:31]([O:33][CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)=[O:32])[C@H:16]1[CH2:21][CH2:20][N:19](C(OC(C)(C)C)=O)[CH2:18][C@H:17]1[O:29][CH3:30])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>CO>[CH2:8]([N:15]([C@H:16]1[CH2:21][CH2:20][NH:19][CH2:18][C@H:17]1[O:29][CH3:30])[C:31](=[O:32])[O:33][CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

Komponenten

4

Edukt 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 86648850tert-Butyl cis(+/-)-4-{benzyl[(benzyloxy)carbonyl]amino}-3-methoxypiperidine-1-carboxylate

Produkt 1

HCID 86712358Benzyl benzyl[cis(+/-)-3-methoxypiperidin-4-yl]carbamate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A 4 N hydrochloric acid/ethyl acetate solution (5 ml, 20 mmol) was added to a solution of tert-butyl cis(±)-4-{benzyl[(benzyloxy)carbonyl]amino}-3-methoxypiperidine-1-carboxylate obtained in Example (259b) (about 1.44 mmol) in methanol (1 mL). The mixture was stirred for one hour and the solvent was evaporated under reduced pressure. The reaction solution was diluted with ethyl acetate, washed with aqueous sodium bicarbonate solution and brine, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The resulting compound was used for the next reaction without purification.

Aufarbeitung

  1. customthe solvent was evaporated under reduced pressure
  2. additionThe reaction solution was diluted with ethyl acetate
  3. washwashed with aqueous sodium bicarbonate solution and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting compound was used for the next reaction without purification

Quellen und Nachweise

ORD-Eintrag
ord-f727394ab29e480296ca03bd394412aa
Quelldatensatz
uspto-grants-2015_01
Patentnummer
US08927588B2

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