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Acetic Anhydride → HCID 20327652、化合物

HRID 258620
ノート
印刷プレビュー

反応式

HRID 258620 の反応式
[OH:1][CH:2]([CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[CH2:3][CH2:4][CH2:5][N:6]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([OH:19])=[O:18])[S:7]([CH3:10])(=[O:9])=[O:8].[C:25](OC(=O)C)(=[O:27])[CH3:26]>C(OCC)C>[C:25]([O:1][CH:2]([CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[CH2:3][CH2:4][CH2:5][N:6]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]([OH:19])=[O:18])[S:7]([CH3:10])(=[O:8])=[O:9])(=[O:27])[CH3:26]
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

4

反応物 2

HCID 7918Acetic AnhydrideHCID 9885481HCID 9885481、化合物

生成物 1

HCID 20327652HCID 20327652、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
60 °C

実験手順

A mixture of 7-[N-4-hydroxynonyl)methanesulfonamido]heptanoic acid (10.9 g., 0.03 mole) (Example 1, Step B) and acetic anhydride (6.1 g., 0.06 mole) is heated at 60° C. for 18 hours. The mixture is cooled and taken up in 80 ml. of ethyl ether. The solution is extracted with an ice-cold solution of 8 g. of sodium hydroxide in 150 ml. of water. The basic solution is separated and acidified with concentrated hydrochloric acid. The crude product that separates is extracted into ether, washed with water and dried over sodium sulfate. The ether is evaporated and the residual oil is purified by chromatography on silica gel using 2% methanol in chloroform as the eluting solvent. There is obtained 7-[N-(4-acetoxynonyl)methanesulfonamido]heptanoic acid as a viscous oil.

後処理

  1. temperatureThe mixture is cooled
  2. extractionThe solution is extracted with an ice-cold solution of 8 g
  3. customThe basic solution is separated
  4. extractionThe crude product that separates is extracted into ether
  5. washwashed with water
  6. dry with materialdried over sodium sulfate
  7. customThe ether is evaporated
  8. customthe residual oil is purified by chromatography on silica gel using 2% methanol in chloroform as the eluting solvent

出典と根拠

ORDレコード
ord-2441191741c9426490e88378889d9aed
出典データセット
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04033996

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