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

HRID 274485
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반응식

HRID 274485 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-27ba2adeb0bf4ba08d9fa642c7d49419
출처 데이터셋
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05389653

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