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

HRID 2416366노트

반응식

HRID 2416366 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-9c38f7096ab2404f90550eb351a0b975
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06824709B2

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