Hydrazine hydrate (1:1) → 5-chloro-2-(3-glycylaminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone hydrate

HRID 614044

반응식

HRID 614044 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:16]2[C:20]([CH3:21])=[N:19][N:18]=[C:17]2[CH2:22][NH:23][C:24](=[O:37])[CH2:25][N:26]2C(=O)C3=CC=CC=C3C2=O)=[C:6]([CH:15]=1)[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:8].O.NN>C(O)C>[OH2:8].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:16]2[C:20]([CH3:21])=[N:19][N:18]=[C:17]2[CH2:22][NH:23][C:24](=[O:37])[CH2:25][NH2:26])=[C:6]([CH:15]=1)[C:7]([C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)=[O:8]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 155678715-chloro-2-[3-(2-phthalimidoacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone

생성물 1

HCID 213257385-chloro-2-(3-glycylaminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone hydrate수율 94%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 5-chloro-2-[3-(2-phthalimidoacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone (2.3 g) in ethanol (20 ml), hydrazine hydrate (0.92 g) is added, and the resultant mixture is refluxed for 1 hour. The precipitated phthalylhydrazide is filtered off, and the filtrate is evaporated under reduced pressure. The residue is dissolved in methylene chloride, washed with saturated aqueous sodium bicarbonate and water in order, dried over sodium sulfate, and evaporated under reduced pressure. The residue is chromatographed on a column of silica gel, and the product obtained from the eluate by evaporation is recrystallized from ethyl acetate to give 5-chloro-2-(3-glycylaminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone hydrate as crystals melting at 110° to 113° C. The yield is 94%.

후처리

  1. filtrationThe precipitated phthalylhydrazide is filtered off
  2. customthe filtrate is evaporated under reduced pressure
  3. dissolutionThe residue is dissolved in methylene chloride
  4. washwashed with saturated aqueous sodium bicarbonate and water in order
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure
  7. customThe residue is chromatographed on a column of silica gel
  8. customthe product obtained from the
  9. customeluate by evaporation
  10. customis recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-4beb4fc9a79943b8b1fe5c5ca97e00c2
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04143048

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