Methyl iodide → 2'-Methoxy-[1,1';3',1"]terphenyl-5'-carboxylic acid methyl ester

HRID 1280881ノート

反応式

HRID 1280881 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[C:7]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:8]([OH:17])=[C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:10]=1)=[O:4].[C:24]([O-])([O-])=O.[K+].[K+].IC>O>[CH3:1][O:2][C:3]([C:5]1[CH:10]=[C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8]([O:17][CH3:24])=[C:7]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:6]=1)=[O:4]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 543630073,5-Bis-phenyl-4-hydroxybenzoic acid methyl ester

生成物 1

HCID 536767312'-Methoxy-[1,1';3',1"]terphenyl-5'-carboxylic acid methyl ester収率 99%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

At ambient temperature, to a stirred mixture containing 2′-hydroxy-[1,1′;3′,1″]terphenyl-5′-carboxylic acid methyl ester (1.232 g, 4.049 mmol) and K2CO3 (0.6155 g, 4.454 mmol) in N,N-DMF (10.1 mL) was added iodomethane (0.353 mL, 5.67 mmol). After 18 h, the reaction was diluted with H2O (100 mL) and the reaction was stirred vigorously. The resulting precipitate was collected, dissolved in CH2Cl2, dried (K2CO3) and concentrated to give 1.167 g, (99%) of the title compound. 1H NMR (DMSO-d6) δ 3.16 (s, 3H), 3.87 (s, 3H), 7.41-7.53 (m, 6H), 7.58-7.60 (m, 4H), 7.89 (s, 2H).

後処理

  1. customThe resulting precipitate was collected
  2. dissolutiondissolved in CH2Cl2
  3. dry with materialdried (K2CO3)
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-ebfd6671b8934ab09335af801ed7cb35
出典データセット
uspto-grants-2002_09
特許番号
US06451845B1

反応ノート

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