Methacrylic Acid → 3'-(2-Methylacryloyloxy)biphenyl-3-yl 2-methylacrylate

HRID 1877706

反応式

HRID 1877706 の反応式
[C:1]1([C:8]2[CH:13]=[CH:12][CH:11]=[C:10](O)[CH:9]=2)[CH:6]=[CH:5][CH:4]=[C:3]([OH:7])[CH:2]=1.[C:15]([OH:20])(=[O:19])[C:16]([CH3:18])=[CH2:17].C1(N=C=N[CH:30]2[CH2:35][CH2:34]CCC2)CCCCC1.O.O.C(O)(=O)[C:39](O)=[O:40]>C1(C)C=CC=CC=1>[CH3:17][C:16](=[CH2:18])[C:15]([O:20][C:10]1[CH:9]=[C:8]([C:1]2[CH:6]=[CH:5][CH:4]=[C:3]([O:7][C:39](=[O:40])[C:35]([CH3:34])=[CH2:30])[CH:2]=2)[CH:13]=[CH:12][CH:11]=1)=[O:19]

参加物

6

反応物 4

HCID 4093Methacrylic AcidHCID 10868DicyclohexylcarbodiimideHCID 61373Oxalic acid dihydrateHCID 691653,3'-Biphenyldiol

生成物 1

HCID 582396283'-(2-Methylacryloyloxy)biphenyl-3-yl 2-methylacrylate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

5.00 g (26.9 mmol) of biphenyl-3,3′-diol, 9.5 ml (0.112 mol) of methacrylic acid and 0.7 g of N,N-dimethylaminopyridine (DMAP) are initially introduced in 200 ml of toluene, a solution of 23.5 g (0.114 mol) of N,N′-dicyclohexylcarbodiimide is added with ice-cooling, and the mixture is stirred overnight at room temp. After addition of 4.4 g of oxalic acid dihydrate, the batch is stirred for 1 h and filtered, and the filtrate is evaporated. The residue is chromatographed on silica gel with heptane/ethyl acetate (2:1), giving 3′-(2-methylacryloyloxy)biphenyl-3-yl 2-methylacrylate as colourless crystals of m.p. 70° C.

後処理

  1. temperaturecooling
  2. stirringthe batch is stirred for 1 h
  3. filtrationfiltered
  4. customthe filtrate is evaporated
  5. customThe residue is chromatographed on silica gel with heptane/ethyl acetate (2:1)

出典と根拠

ORDレコード
ord-c416173b03af4cec87f3da9ef56b3111
出典データセット
uspto-grants-2012_11
特許番号
US08313669B2

関連ノート

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