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Hydrochloric Acid → methyl N-(2-fluoro-4-chloro-5-cyclohexyloxyphenyl)carbamate

HRID 21484
ノート
印刷プレビュー

反応式

HRID 21484 の反応式
[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([OH:9])=[CH:4][C:3]=1[NH:10][C:11](=[O:14])[O:12][CH3:13].[C:15]1(C)[CH:20]=[CH:19][C:18](S([O:24][CH:25]2[CH2:30][CH2:29][CH2:28][CH2:27][CH2:26]2)(=O)=O)=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+].Cl>[I-].[K+].CN(C)C=O>[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][CH:15]2[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]2)=[CH:4][C:3]=1[NH:10][C:11](=[O:14])[O:12][CH3:13].[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:24][CH:25]2[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30]2)=[CH:4][C:3]=1[NH2:10]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 13722Cyclohexyl p-toluenesulfonateHCID 19042327methyl N-(2-fluoro-4-chloro-5-hydroxyphenyl)carbamate

生成物 2

HCID 152793952-Fluoro-4-chloro-5-cyclohexyloxyanilineHCID 19374473methyl N-(2-fluoro-4-chloro-5-cyclohexyloxyphenyl)carbamate
収率 8.1%

試薬・触媒・溶媒 2

HCID 4875Potassium Iodide溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

Methyl N-(2-fluoro-4-chloro-5-hydroxyphenyl)carbamate (1.00 g, 4.56 mmol) synthesized by the process described in Reference Example 3, cyclohexyl p-toluenesulfonate (1.20 g, 4.73 mmol), potassium carbonate (635 mg, 4.95 mmol), a catalytic amount of potassium iodide and N,N-dimethylformamide (20 ml) as a solvent were charged into a 100 cc round-bottom flask, and stirred on an oil bath at 80° C. After completion of the reaction, the reaction solution was cooled to room temperature, 1N hydrochloric acid (100 ml) was added thereto, and the mixture was extracted with ethyl acetate (20 ml×3). The organic layers were combined, washed with water and a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The drying agent was removed by filtration, the solvent was distilled off under reduced pressure to obtain a crude product (875 mg). The product was isolated and purified by silica gel column chromatography (development solvent: hexane/ethyl acetate=9/1) to obtain methyl N-(2-fluoro-4-chloro-5-cyclohexyloxyphenyl)carbamate (12 mg, 0.46 mmol, 8.1% yield), 2-fluoro-4-chloro-5-cyclohexyloxyaniline (213 mg, 0.87 mmol, 194 yield) and the unreacted starting material, methyl N-(2-fluoro-4-chloro-5-hydroxyphenyl)carbamate (540 mg, 2.46 mmol, 544 recovery ratio). [Methyl N-(2-fluoro-4-chloro-5-cyclohexyloxyphenyl)carbamate] White needle crystals

後処理

  1. customAfter completion of the reaction
  2. temperaturethe reaction solution was cooled to room temperature
  3. extractionthe mixture was extracted with ethyl acetate (20 ml×3)
  4. washwashed with water
  5. dry with materiala saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate
  6. customThe drying agent was removed by filtration
  7. distillationthe solvent was distilled off under reduced pressure
  8. customto obtain a crude product (875 mg)
  9. customThe product was isolated
  10. custompurified by silica gel column chromatography (development solvent: hexane/ethyl acetate=9/1)

出典と根拠

ORDレコード
ord-3d4427abd9114c99ba4001a2231dd2c4
出典データセット
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05424277

反応ノート

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