Water → 8-(2-Furylmethoxy)-8-oxooctyl 2,5-bis[(4-{[6-(acryloyloxy)hexyl]oxy}benzoyl)oxy]benzoate

HRID 424313

反応式

HRID 424313 の反応式
Cl.CN(C)[CH2:4][CH2:5][CH2:6]N=C=NCC.[OH:13][C:14]1[CH:38]=[CH:37][C:36]([OH:39])=[CH:35][C:15]=1[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][C:26]([O:28][CH2:29][C:30]1[O:31][CH:32]=[CH:33][CH:34]=1)=[O:27])=[O:17].C([CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH2:49][O:50][C:51]1[CH:59]=[CH:58][C:54]([C:55]([OH:57])=O)=[CH:53][CH:52]=1)(=O)C=C.[OH2:60]>ClCCl.CN(C)C1C=CN=CC=1>[C:19]([O:18][CH2:16][CH2:15][CH2:14][CH2:38][CH2:37][CH2:36][O:39][C:4]1[CH:5]=[CH:6][C:34]([C:30]([O:13][C:14]2[CH:38]=[CH:37][C:36]([O:39][C:55](=[O:57])[C:54]3[CH:53]=[CH:52][C:51]([O:50][CH2:49][CH2:48][CH2:47][CH2:46][CH2:45][CH2:44][O:28][C:26](=[O:27])[CH:25]=[CH2:24])=[CH:59][CH:58]=3)=[CH:35][C:15]=2[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][C:26]([O:28][CH2:29][C:30]2[O:31][CH:32]=[CH:33][CH:34]=2)=[O:27])=[O:17])=[O:31])=[CH:33][CH:32]=1)(=[O:60])[CH:20]=[CH2:21]

参加物

7

反応物 4

HCID 962WaterHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 22719187HCID 22719187、化合物HCID 590050178-(2-Furylmethoxy)-8-oxooctyl 2,5-dihydroxybenzoate

生成物 1

HCID 590050198-(2-Furylmethoxy)-8-oxooctyl 2,5-bis[(4-{[6-(acryloyloxy)hexyl]oxy}benzoyl)oxy]benzoate

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (4.8 g) in dichloromethane (60 ml) was slowly added to a solution of 8-(2-furylmethoxy)-8-oxooctyl 2,5-dihydroxybenzoate (3.7 g), 4-(6-acryloylhexyloxy)benzoic acid (7.3 g) and 4-dimethylaminopyridine (0.6 g) in dichloromethane (150 ml) at 0° C. The mixture was stirred overnight at room temperature. The resulting solution was then added to water (600 ml) and extracted with dichloromethane (3×200 ml). The combined organic layers were washed with water (2×200 ml), dried over magnesium sulphate and filtered. The solvent removed in vacuum. The residue (10.4 g) was purified by column flash chromatography on silica gel using toluene/ethyl acetate (95:5) as eluent, to give 8-(2-furylmethoxy)-8-oxooctyl 2,5-bis[(4-{[6-(acryloyloxy)hexyl]oxy}benzoyl)oxy]benzoate.

後処理

  1. extractionextracted with dichloromethane (3×200 ml)
  2. washThe combined organic layers were washed with water (2×200 ml)
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. customThe solvent removed in vacuum
  6. customThe residue (10.4 g) was purified by column flash chromatography on silica gel

出典と根拠

ORDレコード
ord-c05dcc7cef6c47b8acfdd0b6b67beead
出典データセット
uspto-grants-2012_01
特許番号
US08105662B2

関連ノート

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