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Dimethylformamide → HCID 14370897、化合物

HRID 2165334
ノート
印刷プレビュー

反応式

HRID 2165334 の反応式
CN([CH:4]=[O:5])C.[CH2:6]([O:18][C:19]1[CH:24]=[CH:23][C:22]([CH2:25][C:26]([OH:28])=[O:27])=[CH:21][CH:20]=1)[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].Br[CH:30]([CH3:34])[C:31](O)=[O:32].[C:35](=O)([O-])[O-].[K+].[K+]>O>[CH2:6]([O:18][C:19]1[CH:24]=[CH:23][C:22]([CH2:25][C:26]([O:28][CH:30]([C:31]([O:5][CH2:4][CH3:35])=[O:32])[CH3:34])=[O:27])=[CH:21][CH:20]=1)[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 117292-Bromopropionic acidHCID 10336152Benzeneacetic acid, 4-(dodecyloxy)-

生成物 1

HCID 14370897HCID 14370897、化合物収率 76%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

To a DMF solution (30 ml) of 4-dodecyloxyphenylacetic acid (2.4 g, 7.5 mmol.) and 2-bromopropionic acid (1.5 g, 8 mmol.) was added potassium carbonate (1.5 g, 10 mmol.). The mixture was stirred at 80° C. for 2 hours. The reaction solution was cooled, to which was added water (50 ml). The mixture was subjected to extraction with IPE. The organic layer was washed with water, dried and concentrated under reduced pressure. The concentrate was purified by means of a silica gel chromatography (developing solvent: IPE) to give 1-ethoxycarbonylethyl 4-dodecyloxyphenylacetate (2-i, 2.4 g, 76%).

後処理

  1. temperatureThe reaction solution was cooled, to which
  2. extractionThe mixture was subjected to extraction with IPE
  3. washThe organic layer was washed with water
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customThe concentrate was purified by means of a silica gel chromatography (developing solvent: IPE)

出典と根拠

ORDレコード
ord-e91a960c508948bd8dff69722ce7e319
出典データセット
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04939274

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート