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Methyl iodide → HCID 21326076, 화합물

HRID 25958
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HRID 25958 반응식
[C:1]([NH:4][NH:5][C:6]1[S:7][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[CH3:17])=[N:9][N:10]=1)(=[O:3])[CH3:2].[Na].[CH3:19]I>C(O)C>[C:1]([N:4]([CH3:19])[NH:5][C:6]1[S:7][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[CH3:17])=[N:9][N:10]=1)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 5360545SodiumHCID 136840272-(2-Acetylhydrazino)-5-(2-methylphenyl)-1,3,4-thiadiazole

생성물 1

HCID 21326076HCID 21326076, 화합물수율 68.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-(2-Acetylhydrazino)-5-(2-methylphenyl)-1,3,4-thiadiazole (6.30 g) was added to a stirred solution of sodium (0.57 g) in ethanol (63 ml) at room temperature. After 15 minutes methyl iodide (7.10 g) was added and the solution kept at room temperature for 31/2 hours. The solvent was removed in vacuo and the residue chromatographed on a silica column (315 g) using mixtures of methanol and chloroform, finally eluting with 5% methanolchloroform. The resultant product was crystallised from ethyl acetate to give 2-(2-acetyl-2-methylhydrazino)-5-(2-methylphenyl)-1,3,4-thiadiazole (4.57 g) m.p. 106°-8°.

후처리

  1. customkept at room temperature for 31
  2. custom2 hours
  3. customThe solvent was removed in vacuo
  4. customthe residue chromatographed on a silica column (315 g)
  5. washfinally eluting with 5% methanolchloroform
  6. customThe resultant product was crystallised from ethyl acetate

출처 및 근거

ORD 기록
ord-d01c492ba6924303b2dda064df2f2ee0
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04147794

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