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Acetic Acid → [4-(5-Chloro-isoquinolin-6-yloxy)-cyclohexyl]-cyclohexyl-amine

HRID 2370737
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2370737
[Cl:1][C:2]1[C:11]([O:12][CH:13]2[CH2:18][CH2:17][C:16](=O)[CH2:15][CH2:14]2)=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][N:6]=[CH:7]2.C(N(CC)CC)C.[CH:27]1([NH2:33])[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]1.C(O)(=O)C.C([BH3-])#N.[Na+]>CO>[Cl:1][C:2]1[C:11]([O:12][CH:13]2[CH2:18][CH2:17][CH:16]([NH:33][CH:27]3[CH2:32][CH2:31][CH2:30][CH2:29][CH2:28]3)[CH2:15][CH2:14]2)=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][N:6]=[CH:7]2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 176Acetic AcidHCID 7965CyclohexylamineHCID 8471TriethylamineHCID 5003444Sodium cyanoborohydrideHCID 592685134-(5-Chloro-isoquinolin-6-yloxy)-cyclohexanone

Produkt 1

HCID 25055878[4-(5-Chloro-isoquinolin-6-yloxy)-cyclohexyl]-cyclohexyl-amine
Ausbeute 53,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

100 mg (0.36 mmol) 4-(5-Chloro-isoquinolin-6-yloxy)-cyclohexanone (79) were dissolved in 10 ml methanol. After adding 73 mg (0.73 mmol) triethyl amine, 108 mg (1.09 mmol) cyclohexylamine, 218 mg (3.63 mmol) acetic acid and freshly dried molecular sieves, the reaction was stirred at room temperature. After 30 minutes, a solution of 68 mg (1.09 mmol) sodium cyanoborohydride in 2 ml methanol was added and the reaction was kept at room temperature until complete conversion was achieved. For working up, the reaction mixture was filtered and the filtrate was brought to alkaline pH by adding solid NaHCO3. After evaporation of the solvent, the residue was taken up in H2O and extracted three times with dichloromethane. The combined organic layers were dried over MgSO4 and evaporated. Final purification by preparative HPLC gave 69 mg of the desired product as trifluoroacetate, which was dissolved in 2 N HCl and lyophilized, to yield 45 mg of the corresponding HCl-salt. Rt=1.08/1.15 min (Method #1). Detected mass: 359.3/361.3 (M+H+).

Aufarbeitung

  1. customwas kept at room temperature until complete conversion
  2. filtrationthe reaction mixture was filtered
  3. additionby adding solid NaHCO3
  4. customAfter evaporation of the solvent
  5. extractionextracted three times with dichloromethane
  6. dry with materialThe combined organic layers were dried over MgSO4
  7. customevaporated
  8. customFinal purification by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-de6808444b6545f08031604e66d1b1d7
Quelldatensatz
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08710228B2

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