Hydrochloric Acid → 4-{[4-({6-[2-(Acryloyloxy)-1-methylethoxy]-6-oxohexyl}oxy)benzoyl]oxy}-2-methylphenyl 4-({6-[2-(acryloyloxy)-1-methylethoxy]-6-oxohexyl}oxy)benzoate

HRID 424305ノート

反応式

HRID 424305 の反応式
[C:1]([O:5][CH2:6][CH:7]([O:9][C:10](=[O:17])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]Br)[CH3:8])(=[O:4])[CH:2]=[CH2:3].[OH:18][C:19]1[CH:44]=[CH:43][C:22]([C:23]([O:25][C:26]2[CH:31]=[CH:30][C:29]([O:32][C:33](=[O:41])[C:34]3[CH:39]=[CH:38][C:37]([OH:40])=[CH:36][CH:35]=3)=[CH:28][C:27]=2[CH3:42])=[O:24])=[CH:21][CH:20]=1.[C:45]([O-:48])([O-:47])=O.[K+].[K+].Cl>CC(=O)CC>[C:1]([O:5][CH2:6][CH:7]([CH3:8])[O:9][C:10](=[O:17])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][O:18][C:19]1[CH:20]=[CH:21][C:22]([C:23]([O:25][C:26]2[CH:31]=[CH:30][C:29]([O:32][C:33](=[O:41])[C:34]3[CH:39]=[CH:38][C:37]([O:40][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][C:45]([O:48][CH:7]([CH3:8])[CH2:6][O:5][C:1](=[O:4])[CH:2]=[CH2:3])=[O:47])=[CH:36][CH:35]=3)=[CH:28][C:27]=2[CH3:42])=[O:24])=[CH:43][CH:44]=1)(=[O:4])[CH:2]=[CH2:3]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 109921202-Methyl-1,4-phenylene bis(4-hydroxybenzoate)HCID 590050292-[(6-Bromohexanoyl)oxy]propyl acrylate

生成物 1

HCID 590050254-{[4-({6-[2-(Acryloyloxy)-1-methylethoxy]-6-oxohexyl}oxy)benzoyl]oxy}-2-methylphenyl 4-({6-[2-(acryloyloxy)-1-methylethoxy]-6-oxohexyl}oxy)benzoate

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

反応条件

温度
100 °C

実験手順

A mixture of 2-[(6-bromohexanoyl)oxy]propyl acrylate (4.15 g), 4-[(4-hydroxybenzoyl)oxy]-2-methylphenyl 4-hydroxybenzoate (2.24 g) and K2CO3 (2.55 g) in 2-butanone (40 ml) was heated at 100° C. overnight. The reaction mixture was poured into HCl 1N (50 ml) and extracted twice with 80 ml of diethylether. The etheral extracts were dried over Na2SO4 and evaporated to dryness. The obtained pasty residue was purified by silica column chromatography to give nearly pure 4-{[4-({6-[2-(acryloyloxy)-1-methylethoxy]-6-oxohexyl}oxy)benzoyl]oxy}-2-methylphenyl 4-({6-[2-(acryloyloxy)-1-methylethoxy]-6-oxohexyl}oxy)benzoate as slightly yellow oil.

後処理

  1. extractionextracted twice with 80 ml of diethylether
  2. dry with materialThe etheral extracts were dried over Na2SO4
  3. customevaporated to dryness
  4. customThe obtained pasty residue was purified by silica column chromatography

出典と根拠

ORDレコード
ord-c964ac44e6d444afb239752f5154e044
出典データセット
uspto-grants-2012_01
特許番号
US08105662B2

反応ノート

読み込み中…