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2,3-Dihydro-α-methyl-N-(phenylmethyl)-1,4-benzodioxin-2-methanamine → 1,4-Benzodioxan, 2-(1-aminoethyl)-

HRID 1855957
ノート
印刷プレビュー

反応式

HRID 1855957 の反応式
C([NH:8][CH:9]([CH:11]1[O:16][C:15]2[CH:17]=[CH:18][CH:19]=[CH:20][C:14]=2[O:13][CH2:12]1)[CH3:10])C1C=CC=CC=1>CO.Cl.[Pd]>[O:16]1[C:15]2[CH:17]=[CH:18][CH:19]=[CH:20][C:14]=2[O:13][CH2:12][CH:11]1[CH:9]([NH2:8])[CH3:10]
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 1

HCID 5418362,3-Dihydro-α-methyl-N-(phenylmethyl)-1,4-benzodioxin-2-methanamine

生成物 1

HCID 171801,4-Benzodioxan, 2-(1-aminoethyl)-収率 94.5%

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid触媒HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

In 50 ml of methanol was dissolved 7 g of pure N-benzyl-1-(1,4-benzodioxan-2-yl)ethylamine (i1 '). After adding one drop of ethanolic hydrochloric acid and 0.5 g of 10% palladium charcoal to the solution, and catalytic reduction was performed at normal pressure until the absorption of hydrogen gas stopped. Then, palladium charcoal was filtered away, the filtrate was acidified with the addition of ethanolic hydrochloric acid, and the solvent was distilled off. Then, 20 ml of isopropanol was added to the residue and the product formed was recovered by filtration to provide 4.4 g (75.7%) of 1-(1,4-benzodioxan-2-yl)ethylamine (i1 ') hydrochloride having a melting point of 234°-235° C. The product was then converted into a base by a conventional manner and distilled under reduced pressure to provide 2.9 g (62.3%) of 1-(1,4-benzodioxan-2-yl)ethylamine (i1 ') having a boiling point of 88°-90° C./0.1 mmHg.

後処理

  1. customwas performed at normal pressure until the absorption of hydrogen gas
  2. filtrationThen, palladium charcoal was filtered away
  3. additionthe filtrate was acidified with the addition of ethanolic hydrochloric acid
  4. distillationthe solvent was distilled off
  5. additionThen, 20 ml of isopropanol was added to the residue
  6. customthe product formed
  7. filtrationwas recovered by filtration

出典と根拠

ORDレコード
ord-46edf05f45fe46549779640ceeed34e2
出典データセット
uspto-grants-1980_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04217305

反応ノート

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