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Sodium hydride → (4-Fluoro-3-trifluoromethyl-benzyl)-(3-methyl-benzo[b]thiophen-2-yl)-carbamic acid tert-butyl ester

HRID 2089714
ノート
印刷プレビュー

反応式

HRID 2089714 の反応式
[C:1]([O:5][C:6](=[O:18])[NH:7][C:8]1[S:12][C:11]2[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=2[C:9]=1[CH3:17])([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].[F:21][C:22]1[CH:29]=[CH:28][C:25]([CH2:26]Br)=[CH:24][C:23]=1[C:30]([F:33])([F:32])[F:31]>CN(C=O)C>[C:1]([O:5][C:6](=[O:18])[N:7]([CH2:26][C:25]1[CH:28]=[CH:29][C:22]([F:21])=[C:23]([C:30]([F:33])([F:31])[F:32])[CH:24]=1)[C:8]1[S:12][C:11]2[CH:13]=[CH:14][CH:15]=[CH:16][C:10]=2[C:9]=1[CH3:17])([CH3:4])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 27375774-Fluoro-3-(trifluoromethyl)benzyl bromideHCID 57920379Tert-butyl-3-methylbenzo[b]thiophen-2-ylcarbamate

生成物 1

HCID 59376673(4-Fluoro-3-trifluoromethyl-benzyl)-(3-methyl-benzo[b]thiophen-2-yl)-carbamic acid tert-butyl ester

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of compound 6-B (2.0 g, 7.59 mmol) in DMF (20 mL), cooled to 0° C., was added 60% NaH (0.334 g, 8.35 mmol) and the reaction mixture was stirred for 15 minutes. 4-Fluoro-3-trifluoromethyl benzyl bromide (1.26 mL, 8.35 mmol) was added drop-wise at 0° C. and the reaction mixture was stirred for 1 hour. The reaction mixture was poured into ice water, extracted with ethyl acetate, the organic phase washed with H2O, brine, dried over MgSO4, filtered, and the solvent evaporated under reduced pressure. The crude oil was purified by flash column chromatography (SiO2) eluting with a 0% EtOAc-heptane to 25% EtOAc-heptane gradient to afford compound 6-C as a clear oil. Compound 6-C was used without further purification in the next step.

後処理

  1. stirringthe reaction mixture was stirred for 1 hour
  2. extractionextracted with ethyl acetate
  3. washthe organic phase washed with H2O, brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe solvent evaporated under reduced pressure
  7. customThe crude oil was purified by flash column chromatography (SiO2)
  8. washeluting with a 0% EtOAc-heptane to 25% EtOAc-heptane gradient

出典と根拠

ORDレコード
ord-4a4c2297a53a463d9d16eef958633258
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436041B2

反応ノート

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