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Ethanamine, 2-(2-methoxyethoxy)-N,N-bis[2-(2-methoxyethoxy)ethyl]- → HCID 22107237、化合物

HRID 1456679
ノート
印刷プレビュー

反応式

HRID 1456679 の反応式
Cl[C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([O-:6])=[O:5].[Na+].[CH:12]1([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[O-:24])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1.[Na+].COCCOCCN(CCOCCOC)CCOCCOC>COCCOCCOC.[Cu]Cl>[CH:12]1([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[O:24][C:2]2[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=2[C:4]([OH:6])=[O:5])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 112414Ethanamine, 2-(2-methoxyethoxy)-N,N-bis[2-(2-methoxyethoxy)ethyl]-HCID 23663665Sodium o-chlorobenzoateHCID 23684558Sodium 2-cyclohexylphenolate

生成物 1

HCID 22107237HCID 22107237、化合物収率 68%

試薬・触媒・溶媒 2

HCID 62652Cuprous chloride触媒
HCID 8150
Diglyme
溶媒

実験手順

A mixture of 21.4 g (0.12 mol) of sodium 2-chlorobenzoate, 26.1 g (0.132 mol) of sodium 2-cyclohexylphenolate, 4.95 g (0.05 mol) of copper(I) chloride and 16.17 g (0.05 mol) of tris[2-(2-methoxyethoxy)-ethyl]amine (TDA) in 1.5 l of diethylene glycol dimethyl ether ("diglyme") is kept at 140° C. for 8 hours. The solvent is then concentrated on a vacuum rotary evaporator and the residue is diluted with water and acidified with concentrated hydrochloric acid. The product is extracted with ethyl acetate. The organic phases are washed with water, combined, dried over sodium sulfate and concentrated on a vacuum rotary evaporator. 22.2 g (68%) of 2-(2-cyclohexylphenoxy)benzoic acid, melting point 109°-123° C., result as a beige powder.

後処理

  1. concentrationThe solvent is then concentrated on a vacuum rotary evaporator
  2. additionthe residue is diluted with water
  3. extractionThe product is extracted with ethyl acetate
  4. washThe organic phases are washed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated on a vacuum rotary evaporator

出典と根拠

ORDレコード
ord-49ec1f354ccc45f8a5eda9c0f80c252a
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05844024

反応ノート

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