Diethanolamine → 2-[6-(Bis(2-hydroxyethyl)amino)hexyl-(2-hydroxyethyl)amino]ethanol

HRID 321921ノート

反応式

HRID 321921 の反応式
[CH2:1]([NH:4][CH2:5][CH2:6][OH:7])[CH2:2][OH:3].Br[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14]Br.[OH-:16].[Na+]>CO>[OH:3][CH2:2][CH2:1][N:4]([CH2:5][CH2:6][OH:7])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][N:4]([CH2:1][CH2:2][OH:3])[CH2:5][CH2:6][OH:16]

参加物

5

反応物 3

HCID 8113DiethanolamineHCID 123681,6-DibromohexaneHCID 14798Sodium Hydroxide

生成物 1

HCID 2297292-[6-(Bis(2-hydroxyethyl)amino)hexyl-(2-hydroxyethyl)amino]ethanol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
57.5 °C

実験手順

N,N-Diethanolamine (1331.3 g, 11.36 mol) is placed in a 5000 ml three-necked round bottomed flask fitted with a condenser, addition funnel, internal thermometer, mechanical stirrer and argon inlet. 1,6-Dibromohexane (1386 g, 5.68 mol) is added via the addition funnel slowly to keep the reaction temperature below 60° C. After addition is completed the mixture is heated to 55-60° C. for 18 h. The reaction mixture is poured into a 6 L Erlenmeyer flask containing a solution of methanol (1.5 L) and sodium hydroxide (227.2 g, 5.68 mol). White salts begin to precipitate. After 4 h, the mixture is filtered. The filtrate is concentrated under reduced pressure to leave the product as a viscous oil.

後処理

  1. customfitted with a condenser, addition funnel
  2. customthe reaction temperature below 60° C
  3. additionAfter addition
  4. additionThe reaction mixture is poured into a 6 L Erlenmeyer flask
  5. customto precipitate
  6. filtrationthe mixture is filtered
  7. concentrationThe filtrate is concentrated under reduced pressure

出典と根拠

ORDレコード
ord-0c32e3622a20475282538655b81ea390
出典データセット
uspto-grants-2001_04
特許番号
US06211140B1

反応ノート

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