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Hydrazinium chloride → 1-Hydrazino-3,4-dihydroisoquinoline hydrochloride

HRID 436431
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HRID 436431 반응식
C(O[C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7][CH2:6][N:5]=1)C.[ClH:14].[NH2:15][NH2:16]>C(O)C>[ClH:14].[NH:15]([C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7][CH2:6][N:5]=1)[NH2:16]
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참가 물질

4

반응물 2

HCID 115031Hydrazinium chlorideHCID 123490381-Ethoxy-3,4-dihydroisoquinoline

생성물 1

HCID 214525621-Hydrazino-3,4-dihydroisoquinoline hydrochloride수율 79.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1-ethoxy-3,4-dihydroisoquinoline (1.0 g.), hydrazine monohydrochloride (0.4 g.) and absolute ethanol (15 ml.) was heated under reflux (for 40 min.). The solution was cooled, filtered and concentrated and the residue was recrystallized from ethanol-ether, affording 1-hydrazino-3,4-dihydroisoquinoline hydrochloride (0.9 g., m.p. 205°-207° C.). C. A mixture of 1-hydrazino-3,4-dihydroisoquinoline (8.0 g.), acetaldehyde (20 ml.) and ethanol (20 ml.) was allowed to stand at room temperature (for 45 min). Ethanolic sulfuric acid was added until the solution was distinctly acidic. Ether was added. The resulting oil crystallized and the crystals were recrystallized from ethanol-ether, affording 1-(2-ethylidenehydrazino)-3,4-dihydroisoquinoline (I: X=CH3, X'=Y=Y'=Z=Z'=H) sulfate in two crops (8.3 g., m.p. 152°-154° C.; 0.5 g., m.p. 152°-155° C.).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux (for 40 min.)
  3. temperatureThe solution was cooled
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customthe residue was recrystallized from ethanol-ether

출처 및 근거

ORD 기록
ord-2fe5d4827699491496fd61f7c51c25e5
출처 데이터셋
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04009170

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