Hydrochloric Acid → Hydrazine, (4-chlorophenyl)methyl-

HRID 736281노트

반응식

HRID 736281 반응식
C(=[N:14][N:15]([C:17]1[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=1)[CH3:16])(C1C=CC=CC=1)C1C=CC=CC=1.Cl.[OH-].[Na+]>O1CCCC1>[Cl:23][C:20]1[CH:21]=[CH:22][C:17]([N:15]([CH3:16])[NH2:14])=[CH:18][CH:19]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86620834N'-Benzhydrylidene-N-(4-chlorophenyl)-N-methylhydrazine

생성물 1

HCID 11182748Hydrazine, (4-chlorophenyl)methyl-

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

N′-Benzhydrylidene-N-(4-chlorophenyl)-N-methylhydrazine (1.5 g, 4.68 mmol) is placed in 20 mL of tetrahydrofuran with stirring. 5 mL of 5 N hydrochloric acid are added thereto and the solution is then left stirring at a temperature in the region of 50° C. for 16 hours. The aqueous phase is then neutralized with 5 N sodium hydroxide and is then extracted with ethyl acetate. The oil obtained after extraction is purified by chromatography on silica gel, eluting at the start with an ethyl acetate/heptane mixture (10/90 by volume). N-(4-Chlorophenyl)-N-methylhydrazine is thus obtained in the form of a pale yellow oil, 0.53 g (72%). (Rf=0.48. 20/80 EtOAc/heptane (v/v)).

후처리

  1. waitthe solution is then left
  2. stirringstirring at a temperature in the region of 50° C. for 16 hours
  3. extractionis then extracted with ethyl acetate
  4. customThe oil obtained
  5. extractionafter extraction
  6. customis purified by chromatography on silica gel
  7. washeluting at the start with an ethyl acetate/heptane mixture (10/90 by volume)

출처 및 근거

ORD 기록
ord-6b5dc2cdbedf4be9a47534ca9532e3d1
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07595320B2

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