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Acetic Anhydride → 3-Acetoxy-5-hydroxy-4-phenylazo-benzoic acid methyl ester

HRID 414523
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인쇄 미리보기

반응식

HRID 414523 반응식
[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[C:8]([OH:10])[C:7]([N:11]=[N:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:6]([OH:19])[CH:5]=1.[C:21](OC(=O)C)(=[O:23])[CH3:22]>C(O)(=O)C>[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[C:8]([OH:10])[C:7]([N:11]=[N:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:6]([O:19][C:21](=[O:23])[CH3:22])[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 1360597863,5-Dihydroxy-4-phenylazo-benzoic acid methyl ester

생성물 1

HCID 1361762643-Acetoxy-5-hydroxy-4-phenylazo-benzoic acid methyl ester

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 27 g. of 3,5-dihydroxy-4-phenylazo-benzoic acid methyl ester, 250 ml. of glacial acetic acid and 21 g. of acetic anhydride was stirred at 100° C. for 3 hours, complete solution occurring. The resulting solution was evaporated to dryness under reduced pressure. The residue was taken up in methanol and again evaporated to dryness. The residue was recrystallized from dimethylformamide/methanol and there was obtained 3-acetoxy-5-hydroxy-4-phenylazo-benzoic acid methyl ester having a melting point of 162° C.

후처리

  1. additionA mixture of 27 g
  2. customThe resulting solution was evaporated to dryness under reduced pressure
  3. customagain evaporated to dryness
  4. customThe residue was recrystallized from dimethylformamide/methanol

출처 및 근거

ORD 기록
ord-d88ef3528c3d4020bb59912c19ba67d8
출처 데이터셋
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04792557

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