Oxygen → HCID 86754079、化合物

HRID 1075700ノート

反応式

HRID 1075700 の反応式
[C:1]([NH:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9][O:10][CH2:11][CH2:12][OH:13])(=[O:3])[CH3:2].[O:14]=O.[OH-].[Na+:17]>O.[Pd]>[C:1]([NH:4][CH2:5][CH2:6][O:7][CH2:8][CH2:9][O:10][CH2:11][C:12]([O-:14])=[O:13])(=[O:3])[CH3:2].[Na+:17]

参加物

6

反応物 3

HCID 977OxygenHCID 14798Sodium HydroxideHCID 53765498N-{2-[2-(2-Hydroxyethoxy)ethoxy]ethyl}acetamide

生成物 1

HCID 86754079HCID 86754079、化合物収率 94%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

95.5 g of 8-acetylamino-3,6-dioxa-1-octanol were dissolved in 405 g of water, and 2.90 g of Pd/C (10% by weight) were added. The solution was heated to 70° C. and, while stirring vigorously, about 17 ml/min O2 were passed continously through the solution under atmospheric pressure for 14 h. Throughout the reaction, the pH was kept at 10 by continuously metering in a total of 105 g of 20% by weight aqueous NaOH. The remaining solution was then extracted with ethyl acetate in a perforator for 3 days. The aqueous phase was then distilled to dryness to leave 106 g (corresponding to 94% of theory) of sodium 8-acetylamino-3,6-dioxaoctanoate as viscous oil.

後処理

  1. customThroughout the reaction
  2. extractionThe remaining solution was then extracted with ethyl acetate in a perforator for 3 days
  3. distillationThe aqueous phase was then distilled to dryness

出典と根拠

ORDレコード
ord-3c886546e77e41e59c2f078c820bc5ff
出典データセット
uspto-grants-1999_05
特許番号
US05907055

反応ノート

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