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Ethanamine, 2-(2-methoxyethoxy)-N,N-bis[2-(2-methoxyethoxy)ethyl]- → HCID 22107237, 화합물

HRID 726764
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HRID 726764 반응식
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>[Cu]Cl.COCCOCCOC>[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
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참가 물질

6

반응물 3

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

생성물 1

HCID 22107237HCID 22107237, 화합물수율 68%

시약·촉매·용매 2

HCID 62652Cuprous chloride촉매
HCID 8150
Diglyme
용매

실험 절차

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 1 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.

후처리

  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

출처 및 근거

ORD 기록
ord-c6a1053f130b483b8d7e9bf6c035a9d1
출처 데이터셋
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05710198

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