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Sodium Hydroxide → HCID 15453776, 화합물

HRID 1108610
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HRID 1108610 반응식
[CH3:1][N:2]([CH3:23])[CH2:3][CH2:4][O:5][CH:6]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:7]1[CH:12]=[CH:11][C:10]([C:13]([O:15]C)=[O:14])=[CH:9][CH:8]=1.[OH-].[Na+]>CO.Cl>[CH3:1][N:2]([CH3:23])[CH2:3][CH2:4][O:5][CH:6]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:7]1[CH:12]=[CH:11][C:10]([C:13]([OH:15])=[O:14])=[CH:9][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 22320094HCID 22320094, 화합물

생성물 1

HCID 15453776HCID 15453776, 화합물수율 87%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 887Methanol용매

실험 절차

0.53 g(1.69 mmol) of methyl α-(2-dimethylaminoethoxy)-α-phenyl-p-toluate) was dissolved in 10 ml of methanol. 2.54 ml of a 1N sodium hydroxide aqueous solution was added thereto and the mixture was refluxed under heating for 1 hour. After the reaction mixture was cooled, 2.54 ml of IN hydrochloric acid was added thereto and the mixture was concentrated to dryness. A mixture of chloroform and methanol (5:1 (v/v)) was added to the residue, and the resulting mixture was stirred for a while, then filtered with Celite. The solvent was distilled off and the residue was triturated with diethyl ether. The resulting precipitate was collected by filtration to obtain 0.44 g (1.47 mmol) of α-(2-dimethylaminoethoxy)-α-phenyl-p-toluic acid as pale yellow brown powder. ##STR11## Its spectroscopic data are as follows: 1H-NMR (CDCl1) δ (ppm) 2.62 (6H, s), 3.00 (2H, m), 3.59 (1H, m), 3.82 (1H, m), 5.37 (1H, s), 7.21~7.36 (7H, m), 7.77 (2H, d, J=8.4 Hz).

후처리

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 1 hour
  3. temperatureAfter the reaction mixture was cooled
  4. concentrationthe mixture was concentrated to dryness
  5. additionA mixture of chloroform and methanol (5:1 (v/v))
  6. additionwas added to the residue
  7. filtrationfiltered with Celite
  8. distillationThe solvent was distilled off
  9. customthe residue was triturated with diethyl ether
  10. filtrationThe resulting precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-cb47a84262d243ae919973dc22363e84
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06069149

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