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

HRID 1183611
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HRID 1183611 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

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

생성물 1

HCID 687331102-(3-Amino-4-cyclopropylmethoxy-5-trifluoromethyl-phenyl)-4-methyl-pentanoic acid ethyl ester수율 51.3%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 313Hydrochloric Acid
용매
HCID 702Ethanol용매

실험 절차

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, 1H), 4.04 (m, 2H), 3.85 (s, 2H), 3.66 (d, 2H, J=6.9 Hz), 3.45 (t, 1H, J=7.8 Hz), 1.84 (m, 1H), 1.49 (m, 1H), 1.39 (m, 1H), 1.22 (m, 1H), 1.14 (t, 3H, J=7.2 Hz), 0.82 (m, 6H), 0.56 (d, 2H, J=7.5 Hz), 0.27 (d, 2H, 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.

후처리

  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)

출처 및 근거

ORD 기록
ord-8036cd126782447990392d4d8947c625
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08664249B2

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