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Acetohydrazide → HCID 20350618, 화합물

HRID 614200
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HRID 614200 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10](SC)[N:9]([CH3:14])[N:8]=[C:7]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[C:6]=2[CH:21]=1.[C:22]([NH:25][NH2:26])(=O)[CH3:23]>C(O)CCC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[C:22]([CH3:23])=[N:25][N:26]=[C:10]3[N:9]([CH3:14])[N:8]=[C:7]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[C:6]=2[CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14039AcetohydrazideHCID 6287943H-1,3,4-Benzotriazepine, 7-chloro-3-methyl-2-(methylthio)-5-phenyl-

생성물 1

HCID 20350618HCID 20350618, 화합물

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

A mixture of 7.25 grams (23.0 m moles) of 7-chloro-3-methyl-(methylthio)-5-phenyl-3H-1,3,4-benzotriazepine (Example 27), 4.8 grams (65 moles) of acethydrazide, and 100 ml of n-butanol was stirred and refluxed under nitrogen for about 17 hours. The solvent was removed in vacuo on a rotary evaporator. The residue was dissolved in methylene chloride. The resulting solution was washed with water, dried with magnesium sulfate, and concentrated in vacuo. The residue was dissolved in a minimum amount of warm carbon tetrachloride. The solution was cooled and seeded with product. The precipitate was collected, washed with cold carbon tetrachloride, and air dried to yield the title compound as a yellow solid. The melting point was found to be 224.5°-227.5° C. The structure was confirmed by elemental analysis.

후처리

  1. temperaturerefluxed under nitrogen for about 17 hours
  2. customThe solvent was removed in vacuo on a rotary evaporator
  3. dissolutionThe residue was dissolved in methylene chloride
  4. washThe resulting solution was washed with water
  5. dry with materialdried with magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. dissolutionThe residue was dissolved in a minimum amount of warm carbon tetrachloride
  8. temperatureThe solution was cooled
  9. customThe precipitate was collected
  10. washwashed with cold carbon tetrachloride, and air
  11. customdried

출처 및 근거

ORD 기록
ord-f6c28bc81e1643e1a30077ef0805e824
출처 데이터셋
uspto-grants-1979_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04144233

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