Pyridine → alpha-Chlorobenzyl 2-(2-(2-methoxyethoxy)-ethoxy)-ethyl carbonate

HRID 1060788ノート

反応式

HRID 1060788 の反応式
Cl[C:2]([O:4][CH:5]([Cl:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:3].[CH3:13][O:14][CH2:15][CH2:16][O:17][CH2:18][CH2:19][O:20][CH2:21][CH2:22][OH:23].N1C=CC=CC=1>ClCCl>[C:2](=[O:3])([O:23][CH2:22][CH2:21][O:20][CH2:19][CH2:18][O:17][CH2:16][CH2:15][O:14][CH3:13])[O:4][CH:5]([Cl:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 8178Triethylene glycol monomethyl etherHCID 14320655Chloro(phenyl)methyl carbonochloridate

生成物 1

HCID 18629469alpha-Chlorobenzyl 2-(2-(2-methoxyethoxy)-ethoxy)-ethyl carbonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

α-Chlorobenzyl chloroformate (1 g) was added to an ice-cold solution of triethyleneglycol monomethylether (0.7 ml) in dichloromethane (5 ml) followed by pyridine (0.43 ml) at such a rate that the temperature was kept below 10° C. After stirring overnight at room temperature the reaction mixture was washed twice with 0.5 M HCl followed by water and aqueous sodium bicarbonate. Drying over magnesium sulfate, filtration, evaporation in vacuo followed by chromatography on silica gel with hexane/ethyl acetate (1:1) as eluent gave the title compound as a colourless oil.

後処理

  1. customwas kept below 10° C
  2. washwas washed twice with 0.5 M HCl
  3. dry with materialDrying over magnesium sulfate, filtration, evaporation in vacuo

出典と根拠

ORDレコード
ord-080662160f984ae08f0ed276d20d9278
出典データセット
uspto-grants-2003_02
特許番号
US06525077B2

反応ノート

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