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Sodium Hydroxide → 2-Chloro-3-hydroxy-5-nitro-p-anisaldehyde

HRID 274485
ノート
印刷プレビュー

反応式

HRID 274485 の反応式
C([O:4][C:5]1[C:10]([O:11][CH3:12])=[C:9]([N+:13]([O-:15])=[O:14])[CH:8]=[C:7]([CH:16]=[O:17])[C:6]=1[Cl:18])(=O)C.[OH-].[Na+]>CO>[Cl:18][C:6]1[C:5]([OH:4])=[C:10]([O:11][CH3:12])[C:9]([N+:13]([O-:15])=[O:14])=[CH:8][C:7]=1[CH:16]=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 144509942-Chloro-3-formyl-6-methoxy-5-nitrophenyl acetate

生成物 1

HCID 144509952-Chloro-3-hydroxy-5-nitro-p-anisaldehyde

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

35.8 g Of 2-chloro-3-formyl-6-methoxy-5-nitrophenyl acetate are dissolved in 300 ml of methanol. After adding 145 ml of 1N sodium hydroxide solution the mixture is stirred at 23° for 1 hour. After evaporation of the methanol, the residue is diluted with ice-water, made acid with 2N hydrochloric acid and extracted twice with 400 ml of ethyl acetate each time. The organic phases are washed with saturated sodium chloride solution, dried over sodium sulfate and evaporated. The residue is recrystallized from methylene chloride/petroleum ether. There is obtained 2-chloro-3-hydroxy-5-nitro-p-anisaldehyde of m.p. 130°.

後処理

  1. customAfter evaporation of the methanol
  2. additionthe residue is diluted with ice-water
  3. extractionextracted twice with 400 ml of ethyl acetate each time
  4. washThe organic phases are washed with saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customThe residue is recrystallized from methylene chloride/petroleum ether

出典と根拠

ORDレコード
ord-27ba2adeb0bf4ba08d9fa642c7d49419
出典データセット
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05389653

反応ノート

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