1,2-Dichloroethane → 2,7-Bis(4-(6-acryloyloxyhexyl)oxybenzoyloxy)-9-methylfluorene

HRID 2416366ノート

反応式

HRID 2416366 の反応式
[OH:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8]([OH:15])=[CH:9][CH:10]=3)[CH:5]([CH3:16])[C:4]=2[CH:3]=1.[C:17]([O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][O:28][C:29]1[CH:37]=[CH:36][C:32]([C:33](O)=[O:34])=[CH:31][CH:30]=1)(=[O:20])[CH:18]=[CH2:19].[CH2:38](Cl)[CH2:39]Cl.ClCCl>CN(C1C=CN=CC=1)C.O>[C:17]([O:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][O:28][C:39]1[CH:38]=[CH:36][C:32]([C:33]([O:1][C:2]2[CH:14]=[CH:13][C:12]3[C:11]4[C:6](=[CH:7][C:8]([O:15][C:33](=[O:34])[C:32]5[CH:36]=[CH:37][C:29]([O:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][O:21][C:17](=[O:20])[CH:18]=[CH2:19])=[CH:30][CH:31]=5)=[CH:9][CH:10]=4)[CH:5]([CH3:16])[C:4]=3[CH:3]=2)=[O:34])=[CH:31][CH:30]=1)(=[O:20])[CH:18]=[CH2:19]

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 6344DichloromethaneHCID 37135654-((6-(Acryloyloxy)hexyl)oxy)benzoic acidHCID 219606279-methyl-9H-fluorene-2,7-diol

生成物 1

HCID 220350072,7-Bis(4-(6-acryloyloxyhexyl)oxybenzoyloxy)-9-methylfluorene収率 10.6%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 962Water溶媒

実験手順

A mixture of 2,7-dihydroxy-9-methylfluorene (0.5 g), 4-(6-acryloyloxyhexyloxy)benzoic acid (1.52 g), EDC (0.99 g), DMAP (5.76 mg) and dichloromethane (30 mL) was stirred at a room temperature for 12 hours. Water was added to the reaction mixture, and the separated organic layer was washed with water and dried on anhydrous magnesium sulfate. The solvent was distilled off from this organic layer under reduced pressure, and the resulting residue was purified by means of column chromatography (silica gel, eluting solvent: toluene/ethyl acetate [95/5]) and recrystallization (ethanol/ethyl acetate) to obtain 2,7-bis(4-(6-acryloyloxyhexyl)oxybenzoyloxy)-9-methylfluorene (0.19 g) of a white solid matter.

後処理

  1. washthe separated organic layer was washed with water
  2. dry with materialdried on anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off from this organic layer under reduced pressure
  4. customthe resulting residue was purified by means of column chromatography (silica gel, eluting solvent: toluene/ethyl acetate [95/5]) and recrystallization (ethanol/ethyl acetate)

出典と根拠

ORDレコード
ord-9c38f7096ab2404f90550eb351a0b975
出典データセット
uspto-grants-2004_11
特許番号
US06824709B2

反応ノート

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