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

HRID 1067317노트

반응식

HRID 1067317 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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) δ3.16 (s, 3H), 3.87 (s, 3H), 7.41-7.53 (m, 6H), 7.58-7.60 (m, 4H), 7.89 (s, 2H).

후처리

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

출처 및 근거

ORD 기록
ord-c387b49d0b3442f29b87d1ae354a9ed2
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248764B1

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