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Hydrochloric Acid → (4-Nitro-2-phenylbenzoyl)methionine 2-trimethylsilylethyl ester

HRID 383127
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HRID 383127 반응식
[CH3:1][O:2][C:3](=[O:27])[C@H:4]([CH2:23][CH2:24][S:25][CH3:26])[NH:5][C:6](=[O:22])[C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][C:8]=1[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[OH-].[Li+].Cl.[CH3:31][Si:32]([CH3:37])([CH3:36])[CH2:33]CO.C(N=C=NC(C)C)(C)C>CO.CN(C)C1C=CN=CC=1.C1COCC1>[CH3:31][Si:32]([CH3:37])([CH3:36])[CH2:33][CH2:1][O:2][C:3](=[O:27])[C@H:4]([CH2:23][CH2:24][S:25][CH3:26])[NH:5][C:6](=[O:22])[C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][C:8]=1[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 313Hydrochloric Acid2회HCID 3939Lithium HydroxideHCID 12734DiisopropylcarbodiimideHCID 180132-(Trimethylsilyl)ethanolHCID 18666764(4-Nitro-2-phenylbenzoyl)methionine methyl ester

생성물 1

HCID 69844218(4-Nitro-2-phenylbenzoyl)methionine 2-trimethylsilylethyl ester
수율 87%

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of (4-nitro-2-phenylbenzoyl)methionine methyl ester (7.69 g, 30 mmol), prepared as in Example 192A and aqueous saturated lithium hydroxide (20 mL) in methanol (50 mL) was refluxed for 6 hours. The reaction mixture was carefully acidified with concentrated hydrochloric acid (10 mL), and extracted with ethyl acetate (4×). The combine extracts were washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was dissolved in dichloromethane (50 mL) and THF (10 mL) and 2-trimethylsilylethanol (3.72 g, 31.5 mmol), 1,3-diisopropylcarbodiimide (5.17 mL, 33 mmol) and 4-dimethylaminopyridine (30 mg) were added sequentially. After 4 hours, aqueous hydrochloric acid (0.1 N, 0.5 mL) was added and the reaction mixture was stirred for another 2 hours. The reaction mixture was then filtered through silica gel (40 g), and the filtrate was concentrated in vacuo. The residue was purified by column chromatography (5% ethyl ether-hexane) to give the title compound (8.90 g, 87%).

후처리

  1. temperaturewas refluxed for 6 hours
  2. extractionextracted with ethyl acetate (4×)
  3. washThe combine extracts were washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. dissolutionThe residue was dissolved in dichloromethane (50 mL)
  8. filtrationThe reaction mixture was then filtered through silica gel (40 g)
  9. concentrationthe filtrate was concentrated in vacuo
  10. customThe residue was purified by column chromatography (5% ethyl ether-hexane)

출처 및 근거

ORD 기록
ord-ab1843c777d9471da79b969d56bedf9e
출처 데이터셋
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06310095B1

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