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

HRID 2083678
ノート
印刷プレビュー

反応式

HRID 2083678 の反応式
[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]
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 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 7918Acetic Anhydride溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-a568b7c1663544618c8ab9f9b867814b
出典データセット
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04086268

反応ノート

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