HRID2416362

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID11

1,2-Dichloroethane

C2H4Cl2

HCID6344

Dichloromethane

CH2Cl2

HCID3713565

4-((6-(Acryloyloxy)hexyl)oxy)benzoic acid

C16H20O5

HCID14938383

9H-Fluorene-2,7-diol

C13H10O2

PRODUCTS

生成物

结构：C=CC(=O)OCCCCCCOc1ccc(C(=O)Oc2ccc3c(c2)Cc2cc(OC(=O)c4ccc(OCCCCCCOC(=O)C=C)cc4)ccc2-3)cc1

HCID22630269

未命名化合物

收率 22.3%

AUXILIARIES

试剂、催化剂与溶剂

催化剂HCID14284

N,N-Dimethylpyridin-4-amine

C7H10N2

溶剂HCID962

Water

H2O

PROCEDURE

实验过程

A mixture of 2,7-dihydroxyfluorene (0.5 g), 4-(6-acryloyloxyhexyloxy)benzoic acid (1.62 g), EDC (1.06 g), DMAP (6.16 mg) and dichloromethane (30 mL) was stirred at a room temperature for 12 hours. Water was added to the reaction mixture to separate an organic layer, and the resulting 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/toluene) to obtain 2,7-bis(4-(6-acryloyloxyhexyl)oxybenzoyloxy)fluorene (0.42 g) of colorless crystal.

WORKUP

后处理

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

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-e0618c384d974f898d908e9202f951e7
来源数据集: uspto-grants-2004_11
DOI: 10.6084/m9.figshare.5104873.v1
专利: US06824709B2
来源说明: uspto-grants-2004_11

反应 SMILES

[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)[CH2:5][C:4]=2[CH:3]=1.[C:16]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][O:27][C:28]1[CH:36]=[CH:35][C:31]([C:32](O)=[O:33])=[CH:30][CH:29]=1)(=[O:19])[CH:17]=[CH2:18].[CH2:37](Cl)[CH2:38]Cl.ClCCl>CN(C1C=CN=CC=1)C.O>[C:16]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][O:27][C:38]1[CH:37]=[CH:35][C:31]([C:32]([O:1][C:2]2[CH:14]=[CH:13][C:12]3[C:11]4[C:6](=[CH:7][C:8]([O:15][C:32](=[O:33])[C:31]5[CH:35]=[CH:36][C:28]([O:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][O:20][C:16](=[O:19])[CH:17]=[CH2:18])=[CH:29][CH:30]=5)=[CH:9][CH:10]=4)[CH2:5][C:4]=3[CH:3]=2)=[O:33])=[CH:30][CH:29]=1)(=[O:19])[CH:17]=[CH2:18]