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

HRID 1855957
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HRID 1855957 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

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

생성물 1

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

시약·촉매·용매 3

HCID 313Hydrochloric Acid촉매HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-46edf05f45fe46549779640ceeed34e2
출처 데이터셋
uspto-grants-1980_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04217305

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