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Ethanolamine → HCID 86737404, 화합물

HRID 355018
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HRID 355018 반응식
[C:1]12[C:14](=[O:15])[O:13][C:11](=O)[C:2]=1[CH2:3][CH2:4][C:5]1[C:10]2=[CH:9][CH:8]=[CH:7][CH:6]=1.[CH2:16]([CH2:18][NH2:19])[OH:17]>C(O)(=O)C>[OH:17][CH2:16][CH2:18][N:19]1[C:11](=[O:13])[C:2]2[CH2:3][CH2:4][C:5]3[C:10]([C:1]=2[C:14]1=[O:15])=[CH:9][CH:8]=[CH:7][CH:6]=3
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 700EthanolamineHCID 1422143,4-Dihydro-1,2-naphthalenedicarboxylic anhydride

생성물 1

HCID 86737404HCID 86737404, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 70 g (0.35 mol) of 3,4-dihydronaphthalene-1,2-dicarboxylic acid anhydride [prepared according to Org. Syntheses, Col., Vol. 2, 194 (1943)] and 23.5 g (0.385 mol) of ethanolamine in 1.7 liters of glacial acetic acid is kept under reflux for 24 hours. The glacial acetic acid is then removed by distillation, the residue is dissolved in 2 liters of absolute ethanol, 50 g of an ion exchanger ("Dowex 50 W" from Fluka AG) are added and the suspension is kept under reflux for 24 hours. The ion exchanger is then filtered off, the ethanol is distilled off and the residue is recrystallised from diethyl ether/ethanol. This yields 61.8 g (73% of theory) of N-(2'-hydroxyethyl)-3,4-dihydronaphthalene-1,2-dicarboximide; melting point 120.5°-121° C.

후처리

  1. temperatureunder reflux for 24 hours
  2. customThe glacial acetic acid is then removed by distillation
  3. dissolutionthe residue is dissolved in 2 liters of absolute ethanol
  4. addition50 g of an ion exchanger ("Dowex 50 W" from Fluka AG) are added
  5. temperatureunder reflux for 24 hours
  6. filtrationThe ion exchanger is then filtered off
  7. distillationthe ethanol is distilled off
  8. customthe residue is recrystallised from diethyl ether/ethanol

출처 및 근거

ORD 기록
ord-6bfebc718fc2489d945c39c8df8fa7cf
출처 데이터셋
uspto-grants-1983_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04377668

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