Hydrochloric Acid → 4-(2-Hydroxyethylamino)-1-dodecyloxy-2-methyl-2-butanol

HRID 1105

反応式

HRID 1105 の反応式
[NH2:1][CH2:2][C:3]([OH:5])=O.[OH-].[Na+].[CH2:8]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24]CC)[CH:9]1[O:11][CH2:10]1.Cl.[CH2:28](O)[CH3:29]>>[OH:5][CH2:3][CH2:2][NH:1][CH2:28][CH2:29][C:9]([CH3:10])([OH:11])[CH2:8][O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24]

参加物

6

反応物 5

HCID 313Hydrochloric AcidHCID 702Ethanol2 回HCID 750GlycineHCID 14798Sodium HydroxideHCID 38190Oxirane, 2-((tetradecyloxy)methyl)-

生成物 1

HCID 196946244-(2-Hydroxyethylamino)-1-dodecyloxy-2-methyl-2-butanol収率 30.7%

反応条件

温度
80 °C

実験手順

A 300-ml two-necked flask equipped with a stirrer was charged with 7.51 g (0.1 mol) of glycine, 8.3 g (0.1 mol) of 48% NaOH and 200 ml of ethanol. While stirring the mixture at 80° C., an ethanol solution of 2.70 g (10 mmol) of tetradecyl glycidyl ether was added, and the resultant mixture was stirred for 3 hours. After ethanol was distilled off under reduced pressure, methanol and hydrochloric acid was added to the mixture to acidify it. The mixture was subjected to extraction with chloroform. The resultant extract was concentrated under reduced pressure, and the residue was then purified by column chromatography on silica gel, thereby obtaining 1.17 g (yield: 30.7%) of the title compound [(IIa-10) hydrochloride].

後処理

  1. customA 300-ml two-necked flask equipped with a stirrer
  2. distillationAfter ethanol was distilled off under reduced pressure, methanol and hydrochloric acid
  3. additionwas added to the mixture
  4. extractionThe mixture was subjected to extraction with chloroform
  5. extractionThe resultant extract
  6. concentrationwas concentrated under reduced pressure
  7. customthe residue was then purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-5d521726c64849569940c6f7bb84cf4f
出典データセット
uspto-grants-1998_03
特許番号
US05723497

関連ノート

読み込み中…