4-(3-Chloropropyl)morpholine → HCID 20303044、化合物

HRID 1732877ノート

反応式

HRID 1732877 の反応式
[CH2:1]([N:3]([CH2:8][CH3:9])[C:4]([NH:6][CH3:7])=[O:5])[CH3:2].[Cl:10][CH2:11][CH2:12][CH2:13][N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1>O1CCOCC1>[ClH:10].[CH2:1]([N:3]([CH2:8][CH3:9])[C:4]([N:6]([CH3:7])[CH2:11][CH2:12][CH2:13][N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1)=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 958344-(3-Chloropropyl)morpholineHCID 135031N,N-Diethyl-N'-methylurea

生成物 1

HCID 20303044HCID 20303044、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

13 g (0.1 mole) of N,N-diethyl-N'methyl urea are dissolved in 100 cc. of anhydrous dioxane. 3.9 g (0.1 mole) of NaNH2 are added thereto and the reaction mixture is heated one hour at reflux. After cooling, 16.4 g (0.1 mole) of N-(3-chloropropyl)morpholine dissolved in 50 cc. of anhydrous dioxane are added thereto dropwise and the reaction mixture is refluxed for 6 hours. After cooling, the precipitated NaCl is filtered off with suction, the filtrate is evaporated and the remaining residue is subjected to fractionated distillation.

後処理

  1. temperaturethe reaction mixture is heated one hour
  2. temperatureat reflux
  3. temperatureAfter cooling
  4. temperaturedropwise and the reaction mixture is refluxed for 6 hours
  5. temperatureAfter cooling
  6. filtrationthe precipitated NaCl is filtered off with suction
  7. customthe filtrate is evaporated
  8. distillationthe remaining residue is subjected to fractionated distillation

出典と根拠

ORDレコード
ord-8bbe7d843dbb45bd82108f180c340889
出典データセット
uspto-grants-1980_12
特許番号
US04239761

反応ノート

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