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[2-(2-Amino-4-chlorophenoxy)phenyl]methanol → [2-(2-Acetamido-4-chlorophenoxy)phenyl]methyl acetate

HRID 1973336
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반응식

HRID 1973336 반응식
[NH2:1][C:2]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:3]=1[O:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[CH2:7][OH:8]>N1C=CC=CC=1.C(OC(=O)C)(=O)C>[C:3]([O:8][CH2:7][C:6]1[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=1[O:4][C:3]1[CH:13]=[CH:14][C:15]([Cl:17])=[CH:16][C:2]=1[NH:1][C:7](=[O:8])[CH3:6])(=[O:4])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 54153355[2-(2-Amino-4-chlorophenoxy)phenyl]methanol

생성물 1

HCID 20357201[2-(2-Acetamido-4-chlorophenoxy)phenyl]methyl acetate

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 7918Acetic Anhydride용매

실험 절차

0.026 Part of 2-(2-amino-4-chlorophenoxy)benzyl alcohol is dissolved in 0.5 part pyridine and 0.5 part by volume acetic anhydride and allowed to stand at room temperature for 16 hours. The solvent is removed by evaporation under a nitrogen atmosphere and the resultant residue chromatographed on 0.6 part silicic acid. Elution with a 5:95 mixture of ethyl acetate-benzene and recrystallization from a mixture of ethyl acetate and benzene affords 2-(2-acetamido-4-chlorophenoxy)benzyl acetate. This compound melts at about 83° - 84° C. and is represented by the following structural formula. ##STR6## Elemental analysis shows C, 61.71%; H, 5.30%; Cl, 10.73%; N, 4.01%. The calculated values are C, 61.17%; H, 4.83%, Cl, 10.62%; and N, 4.20%.

후처리

  1. customThe solvent is removed by evaporation under a nitrogen atmosphere
  2. customthe resultant residue chromatographed on 0.6 part silicic acid
  3. washElution
  4. additionwith a 5:95 mixture of ethyl acetate-benzene and recrystallization
  5. additionfrom a mixture of ethyl acetate and benzene

출처 및 근거

ORD 기록
ord-05ecc5afa10942f7bc4cff5f42b1befb
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03997401

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