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Triethylamine → HCID 69060367, Verbindung

HRID 1821597
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1821597
[F:1][C:2]1[CH:34]=[C:33]([F:35])[CH:32]=[CH:31][C:3]=1[O:4][C:5]1[N:10]=[C:9]2[N:11]([CH2:22][OH:23])[N:12]=[C:13]([C:14]3[CH:19]=[C:18]([F:20])[CH:17]=[CH:16][C:15]=3[F:21])[C:8]2=[C:7]([NH:24][CH2:25][CH2:26][S:27]([CH3:30])(=[O:29])=[O:28])[N:6]=1.[C:36]([NH:43][C@H:44]([C:48](O)=[O:49])[CH:45]([CH3:47])[CH3:46])([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37].CN(C1C=CC=CN=1)C.C(N(CC)CC)C.ClC(OC(C)=C)=O>C(Cl)Cl>[F:1][C:2]1[CH:34]=[C:33]([F:35])[CH:32]=[CH:31][C:3]=1[O:4][C:5]1[N:10]=[C:9]2[N:11]([CH2:22][O:23][C:48](=[O:49])[CH:44]([NH:43][C:36]([O:38][C:39]([CH3:40])([CH3:42])[CH3:41])=[O:37])[CH:45]([CH3:47])[CH3:46])[N:12]=[C:13]([C:14]3[CH:19]=[C:18]([F:20])[CH:17]=[CH:16][C:15]=3[F:21])[C:8]2=[C:7]([NH:24][CH2:25][CH2:26][S:27]([CH3:30])(=[O:28])=[O:29])[N:6]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 8471TriethylamineHCID 218852-DimethylaminopyridineHCID 83693Boc-L-ValineHCID 93846Isopropenyl chloroformateHCID 16117146HCID 16117146, Verbindung

Produkt 1

HCID 69060367HCID 69060367, VerbindungAusbeute 51,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

[6-(2,4-Difluoro-phenoxy)-3-(2,5-difluoro-phenyl)-4-(2-methanesulfonyl-ethylamino)-pyrazolo[3,4-d]pyrimidin-1-yl]-methanol (170 mg, 0.33 mmol) was dissolved in methylene chloride, and Boc-(L)-Valine (216 mg, 0.99 mmol), dimethylamino pyridine (81 mg, 0.66 mmol), and triethylamine (0.23 mL, 1.6 mmol) were added. The reaction mixture was cooled to 0° C. and stirred under nitrogen, and isopropenyl chloroformate (54 uL, 0.49 mmol) was added. The reaction mixture was stirred for 10 minutes and then partitioned between water and methylene chloride. The organic layer was washed with brine, dried (MgSO4), filtered and concentrated under reduced pressure. The residue was purified by flash chromatography through silica (1:1 hexanes/EtOAc) to give 120 mg of 2-tert-butoxycarbonylamino-3-methyl-butyric acid 6-(2,4-difluoro-phenoxy)-3-(2,5-difluoro-phenyl)-4-(2-methanesulfonyl-ethylamino)-pyrazolo[3,4-d]pyrimidin-1-ylmethyl ester as an oil.

Aufarbeitung

  1. stirringThe reaction mixture was stirred for 10 minutes
  2. custompartitioned between water and methylene chloride
  3. washThe organic layer was washed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by flash chromatography through silica (1:1 hexanes/EtOAc)

Quellen und Nachweise

ORD-Eintrag
ord-83307cd99db84c60ab6e5cff4c841983
Quelldatensatz
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07608603B2

Notizen zur Reaktion

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