Dimethyl sebacate → N,N,N',N'-tetrakis(2-hydroxyethyl)sebacamide

HRID 982587

反応式

HRID 982587 の反応式
[C:1]([O:15]C)(=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][C:10]([O:12]C)=O.[NH:17]([CH2:21][CH2:22][OH:23])[CH2:18][CH2:19][OH:20]>>[OH:20][CH2:19][CH2:18][N:17]([CH2:21][CH2:22][OH:23])[C:10](=[O:12])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][C:1]([N:17]([CH2:21][CH2:22][OH:23])[CH2:18][CH2:19][OH:20])=[O:15]

参加物

3

反応物 2

HCID 7829Dimethyl sebacateHCID 8113Diethanolamine

生成物 1

HCID 231267N,N,N',N'-tetrakis(2-hydroxyethyl)sebacamide

反応条件

温度
140 °C

実験手順

A mixture of 57.58 g (0.25 mol) dimethyl sebacate and 157.71 g (1.50 mol) of diethanolamine was heated in a 140° C. bath under nitrogen for 2.5 hrs while collecting the methanol condensate. The reaction mixture was subsequently heated in a 200° C. at reduced pressure (1.5 mm) to distill off excess diethanolamine. The highly viscous oily residue was dissolved in an equal volume of acetone and stirred overnight. The resulting crystalline solid was collected, washed with acetone, and dried. The yield of product was 35.0 g (9.3% of theory); mp=87-98° C.

後処理

  1. customwhile collecting the methanol condensate
  2. temperatureThe reaction mixture was subsequently heated in a 200° C. at reduced pressure (1.5 mm)
  3. distillationto distill off excess diethanolamine
  4. dissolutionThe highly viscous oily residue was dissolved in an equal volume of acetone
  5. customThe resulting crystalline solid was collected
  6. washwashed with acetone
  7. customdried

出典と根拠

ORDレコード
ord-f811ec377c934eb9b5c669d0d761692b
出典データセット
uspto-grants-2005_03
特許番号
US06861192B2

関連ノート

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