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Sodium Carbonate → 2-(3-Amino-4-cyclopropylmethoxy-5-trifluoromethyl-phenyl)-4-methyl-pentanoic acid ethyl ester

HRID 1512399
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1512399
[CH2:1]([O:3][C:4](=[O:28])[CH:5]([C:10]1[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[C:13]([O:20][CH2:21][CH:22]2[CH2:24][CH2:23]2)=[C:12]([N+:25]([O-])=O)[CH:11]=1)[CH2:6][CH:7]([CH3:9])[CH3:8])[CH3:2].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C.Cl.[Pd]>[CH2:1]([O:3][C:4](=[O:28])[CH:5]([C:10]1[CH:15]=[C:14]([C:16]([F:17])([F:18])[F:19])[C:13]([O:20][CH2:21][CH:22]2[CH2:24][CH2:23]2)=[C:12]([NH2:25])[CH:11]=1)[CH2:6][CH:7]([CH3:9])[CH3:8])[CH3:2]
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Komponenten

6

Edukt 2

HCID 10340Sodium CarbonateHCID 579956202-(4-Cyclopropylmethoxy-3-nitro-5-trifluoromethyl-phenyl)-4-methyl-pentanoic acid ethyl ester

Produkt 1

HCID 687331102-(3-Amino-4-cyclopropylmethoxy-5-trifluoromethyl-phenyl)-4-methyl-pentanoic acid ethyl esterAusbeute 51,3 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23938PalladiumKatalysator
HCID 313
Hydrochloric Acid
Lösungsmittel
HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 2-(4-cyclopropylmethoxy-3-nitro-5-trifluoromethyl-phenyl)-4-methyl-pentanoic acid ethyl ester (1.85 g, 4.59 mmol) and Pd/C (1.85 g) in ethanol and 1 N HCl (4.60 mL) was hydrogenated under 36 psi H2 in a Parr apparatus. After 4 h, the reaction mixture was filtered through Celite 521®. The filtrate was concentrated under reduced pressure to give a yellow oil. The residue was treated with an aqueous solution of sodium carbonate (3 g in 100 mL of water) and the resulting solution was extracted with ethyl acetate (100 mL). The organic layer was dried over sodium sulfate and concentrated under reduced pressure to give a brown oil, which was purified by silica-gel flash chromatography eluting with a gradient of heptane/ethyl acetate (from 10:1 to 2:1) to give 2-(3-amino-4-cyclopropylmethoxy-5-trifluoromethyl-phenyl)-4-methyl-pentanoic acid ethyl ester (0.88 g, 51%) as a light pink oil: 1H NMR (300 MHz, CDCl3): δ 6.83 (s, 1H), 6.80 (s, 1 H), 4.04 (m, 2 H), 3.85 (s, 2 H), 3.66 (d, 2 H, J=6.9 Hz), 3.45 (t, 1 H, J=7.8 Hz), 1.84 (m, 1 H), 1.49 (m, 1 H), 1.39 (m, 1 H), 1.22 (m, 1 H), 1.14 (t, 3 H, J=7.2 Hz), 0.82 (m, 6 H), 0.56 (d, 2 H, J=7.5 Hz), 0.27 (d, 2 H, J=4.5 Hz); 13C NMR (75 MHz, CDCl3): δ 173.61, 142.71, 141.25, 135.51, 123.75 (q, J=30 Hz), 123.52 (q, J=271 Hz), 118.46, 115.52 (q, J=5 Hz), 77.88, 60.70, 49.03, 42.53, 25.86, 22.40, 22.31, 14.07, 10.98, 3.19.

Aufarbeitung

  1. filtrationthe reaction mixture was filtered through Celite 521®
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. customto give a yellow oil
  4. extractionthe resulting solution was extracted with ethyl acetate (100 mL)
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customto give a brown oil, which
  8. customwas purified by silica-gel flash chromatography
  9. washeluting with a gradient of heptane/ethyl acetate (from 10:1 to 2:1)

Quellen und Nachweise

ORD-Eintrag
ord-6dae88fae9404c76a6d271e7aa3dd888
Quelldatensatz
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08217064B2

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