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Ethylene Glycol → Ethyl acetate hexane

HRID 581215
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HRID 581215 반응식
Cl.[CH:2]1[C:15]2[C:6](=[N:7][C:8]3[C:13]([C:14]=2NNS(C2C=C[C:24]([CH3:27])=CC=2)(=O)=O)=[CH:12][CH:11]=[CH:10][CH:9]=3)[CH:5]=[CH:4][CH:3]=1.[OH-:28].[Na+].[CH2:30]([OH:33])[CH2:31][OH:32]>O>[CH3:31][O:32][C:5]1[C:6]2[C:15](=[CH:14][C:13]3[C:8]([N:7]=2)=[CH:9][CH:10]=[CH:11][CH:12]=3)[CH:2]=[CH:3][CH:4]=1.[CH3:14][CH2:15][CH2:2][CH2:3][CH2:4][CH3:5].[C:30]([O:33][CH2:24][CH3:27])(=[O:28])[CH3:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 174Ethylene GlycolHCID 14798Sodium HydroxideHCID 86753010N1-9-acridinyl-N2-p-toluenesulfonylhydrazine hydrochloride

생성물 2

HCID 122924034-MethoxyacridineHCID 21226206Ethyl acetate hexane수율 95.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixed solution comprising 124 mg of N1 -9-(4-methoxy)acridinyl-N2 -p-toluenesulfonylhydrazine hydrochloride (18), 40 mg of sodium hydroxide, and 5 ml of ethylene glycol was allowed to react at 100° C. for a period of one hour. After the completion of the reaction, the reacted solution was introduced into water and the product was extracted by ethyl acetate. After ethyl acetate was distilled away, the residue was purified by column chromatography and 57.6 mg of 4-methoxyacridine (19) was obtained as crystals on recrystallization by hexane-ethyl acetate (yield 95.2%).

후처리

  1. customto react at 100° C. for a period of one hour
  2. customAfter the completion of the reaction
  3. extractionthe product was extracted by ethyl acetate
  4. distillationAfter ethyl acetate was distilled away
  5. customthe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-5540965854974b8dac9651972b41a0c4
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05919928

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