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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 21442569, 화합물 → HCID 21442578, 화합물

HRID 328526
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HRID 328526 반응식
[ClH:1].[CH3:2][C:3]([NH2:19])([CH3:18])[C:4]1[CH:9]=[CH:8][C:7]([C:10]#[C:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:6][CH:5]=1>[Pt](=O)=O.CO>[ClH:1].[CH3:18][C:3]([NH2:19])([CH3:2])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:6][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 21442569HCID 21442569, 화합물

생성물 1

HCID 21442578HCID 21442578, 화합물

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 887Methanol용매

실험 절차

A mixture of 0.45 gram of α,α-dimethyl-4-(phenylethynyl) -benzylamine hydrochloride, 61 ml. of absolute methanol, and 163 mg. of platinum dioxide catalyst is hydrogenated at 40 p.s.i. for one hour. The hydrogenation is stopped, the catalyst is removed by filtration, and the methanol is removed by evaporation. The residue is partitioned between benzene and 10% sodium hydroxide solution. The benzene phase is washed well with water, dried over magnesium sulfate, filtered, and the benzene is evaporated. The residual oil is dissolved in ether and treated with ethanolic hydrogen chloride. The precipitate is collected and recrystallized from isopropanol and ether to give α,α-dimethyl-4-phenethylbenzylamine hydrochloride, m.p. 225°-228° C.

후처리

  1. customthe catalyst is removed by filtration
  2. customthe methanol is removed by evaporation
  3. customThe residue is partitioned between benzene and 10% sodium hydroxide solution
  4. washThe benzene phase is washed well with water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customthe benzene is evaporated
  8. dissolutionThe residual oil is dissolved in ether
  9. additiontreated with ethanolic hydrogen chloride
  10. customThe precipitate is collected
  11. customrecrystallized from isopropanol and ether

출처 및 근거

ORD 기록
ord-14e2ee66fd734a82a189e188585e983b
출처 데이터셋
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04017543

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