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Ammonium Chloride → (R)-benzyl-2-(5-(2-(phenylsulfonyl)ethyl)-1H-indole-3-carbonyl)-pyrrolidine-1-carboxylate

HRID 473057
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 473057
[CH2:1]([Mg]Br)[CH3:2].[C:5]1([S:11]([CH2:14][CH2:15][C:16]2[CH:17]=[C:18]3[C:22](=[CH:23][CH:24]=2)[NH:21][CH:20]=[CH:19]3)(=[O:13])=[O:12])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[Cl-].[NH4+:26].[C:27](=[O:30])(O)[O-:28].[Na+].[Cl-].[Na+].[OH2:34]>CCOCC.ClCCl.[Cl-].[Cl-].[Zn+2]>[CH2:15]([O:28][C:27]([N:26]1[CH2:10][CH2:5][CH2:6][C@@H:2]1[C:1]([C:19]1[C:18]2[C:22](=[CH:23][CH:24]=[C:16]([CH2:15][CH2:14][S:11]([C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=3)(=[O:13])=[O:12])[CH:17]=2)[NH:21][CH:20]=1)=[O:34])=[O:30])[C:16]1[CH:17]=[CH:18][CH:22]=[CH:23][CH:24]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 25517Ammonium ChlorideHCID 516892Sodium BicarbonateHCID 461956503-Dealkyl eletriptanHCID 57417360Sodium chloride; waterHCID 178418443HCID 178418443, Verbindung

Produkt 1

HCID 46195789(R)-benzyl-2-(5-(2-(phenylsulfonyl)ethyl)-1H-indole-3-carbonyl)-pyrrolidine-1-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 3007855ZincchlorideKatalysatorHCID 3283Diethyl EtherLösungsmittelHCID 6344DichloromethaneLösungsmittel3×

Reaktionsbedingungen

Temperatur
-20 °C

Versuchsvorschrift

In a separate setup ethyl magnesium bromide (7.0 ml of a 3M solution in ether) was charged slowly to a solution of 5-(2-(phenylsulfonyl)ethyl)-1H-indole (1.0 g, 3.4 mmol) in dichloromethane. The reaction mixture was heated at reflux for 30 min. The reaction was cooled to −20° C. and ZnCl2 followed by the above prepared CBZ-prolinyl acid chloride in dichloromethane was charged slowly to the reaction at −20° C. The resulting solution was stirred at −15 to −25° C. for 10 h. The completion of the reaction was monitored by TLC. The reaction mass was warmed to RT and diluted with 20 ml dichloromethane. The organic layer was sequentially washed sat. ammonium chloride solution, sat. sodium bicarbonate solution and brine. The organic layer was dried over sodium sulphate and concentrated under vacuum to give a pure product in about 40-75% yield. 1H NMR CDCl3 δ=9.85 (bs, NH), 7.92-7.99 (m, 2H), 7.54-7.80 (m, 5H), 7.28-7.43 (m, 4H), 6.78-7.08 (m, 3H), 4.89-5.28 (m, 3H), 3.53-3.80 (m, 2H), 3.25-3.48 (m, 2H), 2.91-3.19 (m, 2H), 1.70-2.35 (m, 4H). ESI Mass (M−H) 515.6, (M+23) 539.2

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 30 min
  3. additionwas charged slowly to the reaction at −20° C
  4. customThe reaction
  5. temperaturemass was warmed to RT
  6. dry with materialThe organic layer was dried over sodium sulphate
  7. concentrationconcentrated under vacuum
  8. customto give a pure product in about 40-75% yield

Quellen und Nachweise

ORD-Eintrag
ord-6f65666ea2ba4c9686d13d08e675f784
Quelldatensatz
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08633239B2

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