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

HRID 424313

반응식

HRID 424313 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c05dcc7cef6c47b8acfdd0b6b67beead
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08105662B2

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