Trifluoroacetic acid → [7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidin-2-yl]-(4-piperazin-1-yl-phenyl)-amine

HRID 2189293Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2189293
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([NH:20][C:21]3[N:22]=[CH:23][C:24]4[CH:29]=[CH:28][N:27]([CH:30]([CH2:33][CH3:34])[CH2:31][CH3:32])[C:25]=4[N:26]=3)=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[CH2:31]([CH:30]([N:27]1[C:25]2[N:26]=[C:21]([NH:20][C:17]3[CH:18]=[CH:19][C:14]([N:11]4[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]4)=[CH:15][CH:16]=3)[N:22]=[CH:23][C:24]=2[CH:29]=[CH:28]1)[CH2:33][CH3:34])[CH3:32]

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 690753604-{4-[7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino]-phenyl}-piperazine-1-carboxylic acid tert-butyl ester

Produkt 1

HCID 58016034[7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidin-2-yl]-(4-piperazin-1-yl-phenyl)-amineAusbeute 99,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 4-{4-[7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino]-phenyl}-piperazine-1-carboxylic acid tert-butyl ester (167 mg, 0.36 mmol) in dichloromethane (3 mL) is added trifluoroacetic acid (1 mL). The reaction mixture is stirred for 1 h and concentrated in vacuo. The residue is diluted with dichloromethane, washed with NaHCO3 solution, dried over Na2SO4, and concentrated in vacuo. Purification by preparative HPLC afforded 130 mg of [7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidin-2-yl]-(4-piperazin-1-yl-phenyl)-amine as a yellowish solid.

Aufarbeitung

  1. concentrationconcentrated in vacuo
  2. additionThe residue is diluted with dichloromethane
  3. washwashed with NaHCO3 solution
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customPurification by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-cacf9f2c559a46caaff31ab1e396297b
Quelldatensatz
uspto-grants-2012_12
Patentnummer
US08324225B2

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