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Hydrochloric Acid → Methyl N-(3-chloro-4-hydroxyphenyl)carbamate

HRID 1597801
ノート
印刷プレビュー

反応式

HRID 1597801 の反応式
[OH-].[Na+].[NH2:3][C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([Cl:11])[CH:5]=1.Cl[C:13]([O:15][CH3:16])=[O:14].Cl>O>[Cl:11][C:6]1[CH:5]=[C:4]([NH:3][C:13](=[O:14])[O:15][CH3:16])[CH:9]=[CH:8][C:7]=1[OH:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6586Methyl chloroformateHCID 14798Sodium HydroxideHCID 775784-Amino-2-chlorophenol

生成物 1

HCID 18932212Methyl N-(3-chloro-4-hydroxyphenyl)carbamate収率 87%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

5 ml of water and 2.5 ml of 10% aqueous sodium hydroxide solution were carefully added to 1.70 g of 4-amino-2-chlorophenol cooled in an ice-water bath and 2 ml of methyl chloroformate were added dropwise to the resulting mixture. The reaction mixture was then stirred for 3 hours at room temperature, at the end of which it was acidified with 4 ml of 2N hydrochloric acid, and the resulting mixture was extracted with methylene; chloride. The resulting extract was washed with water and then dried over anhydrous sodium sulfate. The solvent was then removed by evaporation under reduced pressure to give a crude crystalline solid which was purified by column chromatography through silica gel using a 2:1 by volume mixture of hexane and ethyl acetate as the eluent to give 2.08 g (yield 87%) of the title compound as a pale brown crystalline solid.

後処理

  1. temperaturecooled in an ice-water bath
  2. extractionthe resulting mixture was extracted with methylene
  3. extractionThe resulting extract
  4. washwas washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was then removed by evaporation under reduced pressure
  7. customto give a crude crystalline solid which
  8. customwas purified by column chromatography through silica gel using a 2:1
  9. additionby volume mixture of hexane and ethyl acetate as the eluent

出典と根拠

ORDレコード
ord-2368dd68468a480ea51565699944a8cf
出典データセット
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05736487

反応ノート

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