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Sodium Hydroxide → HCID 15453776、化合物

HRID 1108610
ノート
印刷プレビュー

反応式

HRID 1108610 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 22320094HCID 22320094、化合物

生成物 1

HCID 15453776HCID 15453776、化合物収率 87%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-cb47a84262d243ae919973dc22363e84
出典データセット
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06069149

反応ノート

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