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Hydrazine hydrate (1:1) → Ammonia

HRID 414617
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반응식

HRID 414617 반응식
[C:1]1([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:6]=[CH:5][C:4]([O:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][N:14]2C(=O)C3=CC=CC=C3C2=O)=[CH:3][CH:2]=1.O.NN>C(O)C>[NH3:14].[C:1]1([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH:2]=[CH:3][C:4]([O:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][NH2:14])=[CH:5][CH:6]=1
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참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 21281403HCID 21281403, 화합물

생성물 2

HCID 222AmmoniaHCID 13957284HCID 13957284, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of N-[6-(4-biphenyloxy)hexyl]phthalimide (17 g), ethanol (500 ml) and hydrazine hydrate (10 ml) was heated at reflux for 16 hours, cooled to room temperature, filtered, and evaporated to dryness. The remaining material was stirred with dichloromethane (500 ml), filtered and evaporated to dryness. The crude product was chromatographed on silica gel, eluting with 95:5 dichloromethane:methanolic ammonia, yielding 6-(4-biphenyloxy)-1-aminohexane as an oil, which was converted to the hydrochloride salt, (m.p. 201°-202° C.), according to the method of Example 3.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 16 hours
  3. filtrationfiltered
  4. customevaporated to dryness
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customThe crude product was chromatographed on silica gel
  8. washeluting with 95:5 dichloromethane

출처 및 근거

ORD 기록
ord-d449bae39c3b4816baabf9de9396e4d3
출처 데이터셋
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04792570

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