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 424305노트

반응식

HRID 424305 반응식
[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]

참가 물질

6

반응물 4

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

생성물 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

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c964ac44e6d444afb239752f5154e044
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08105662B2

반응 노트

불러오는 중…