Pyridine → 2-tert-butyl-4-chloro-5-(2-p-toluenesulfonyloxy-1-(4-tert-butylphenyl)-1-ethyl)oxy-3(2H)-pyridazinone

HRID 1392861ノート

反応式

HRID 1392861 の反応式
[C:1]([N:5]1[C:10](=[O:11])[C:9]([Cl:12])=[C:8]([O:13][CH:14]([C:17]2[CH:22]=[CH:21][C:20]([C:23]([CH3:26])([CH3:25])[CH3:24])=[CH:19][CH:18]=2)[CH2:15][OH:16])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].N1C=CC=C[CH:28]=1.[C:33]1(C)[C:34]([S:39](Cl)(=[O:41])=[O:40])=[CH:35][CH:36]=[CH:37][CH:38]=1>C(OCC)(=O)C>[C:1]([N:5]1[C:10](=[O:11])[C:9]([Cl:12])=[C:8]([O:13][CH:14]([C:17]2[CH:18]=[CH:19][C:20]([C:23]([CH3:26])([CH3:25])[CH3:24])=[CH:21][CH:22]=2)[CH2:15][O:16][S:39]([C:34]2[CH:33]=[CH:38][C:37]([CH3:28])=[CH:36][CH:35]=2)(=[O:40])=[O:41])[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 1049PyridineHCID 8623o-Toluenesulfonyl chlorideHCID 671003162-tert-butyl-4-chloro-5-(2-hydroxy-1-(4-tert-butylphenyl)-1-ethyl)oxy-3(2H)-pyridazinone

生成物 1

HCID 866003922-tert-butyl-4-chloro-5-(2-p-toluenesulfonyloxy-1-(4-tert-butylphenyl)-1-ethyl)oxy-3(2H)-pyridazinone

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a 15 ml round bottom flask charged with 2-tert-butyl-4-chloro-5-(2-hydroxy-1-(4-tert-butylphenyl)-1-ethyl)oxy-3(2H)-pyridazinone (0.25 g, 0.66 mmol) is added pyridine. Toluenesulfonyl chloride (0.15 g, 0.79 mmol) is then added to it and the mixture stirred for 4 hours. The reaction mixture is diluted with ethyl acetate, washed with 5% copper sulfate solution and then with water and dried. After removing the solvent on the rotary evaporator the crude is purified by flash chromatography using ethyl acetate-hexanes as the eluting mixture.

後処理

  1. washwashed with 5% copper sulfate solution
  2. dry with materialwith water and dried
  3. customAfter removing the solvent
  4. customon the rotary evaporator the crude
  5. customis purified by flash chromatography

出典と根拠

ORDレコード
ord-5ef632fc54914083a8c8f2bc3634c703
出典データセット
uspto-grants-2008_03
特許番号
US07344702B2

反応ノート

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