Acetic Anhydride → 2-n-Tridecyl-5-[2-(1-methyl-5-nitroimidazol-2-yl)-vinyl]-1,3,4-thiadiazole

HRID 1856195노트

반응식

HRID 1856195 반응식
[CH2:1]([C:14]1[S:15][C:16]([CH3:19])=[N:17][N:18]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].[CH3:20][N:21]1[C:25]([N+:26]([O-:28])=[O:27])=[CH:24][N:23]=[C:22]1[CH:29]=O.C(OC(=O)C)(=O)C>C(O)(=O)C.[Cl-].[Zn+2].[Cl-]>[CH2:1]([C:14]1[S:15][C:16]([CH:19]=[CH:29][C:22]2[N:21]([CH3:20])[C:25]([N+:26]([O-:28])=[O:27])=[CH:24][N:23]=2)=[N:17][N:18]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]

참가 물질

6

반응물 3

HCID 7918Acetic AnhydrideHCID 784871-Methyl-5-nitro-1H-imidazole-2-carbaldehydeHCID 233463742-Methyl-5-tridecyl-1,3,4-thiadiazole

생성물 1

HCID 537391862-n-Tridecyl-5-[2-(1-methyl-5-nitroimidazol-2-yl)-vinyl]-1,3,4-thiadiazole수율 56.6%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 176Acetic Acid용매

실험 절차

8.45 g of 2-tridecyl-5-methyl-1,3,4-thiadiazole, 4.65 g of 1-methyl-5-nitroimidazole-2-carboxaldehyde and 0.5 g of zinc chloride are heated in 40 ml of acetic acid and 15 ml of acetic anhydride for 24 hours at reflux temperature. After the solvent has been removed, the residue is recrystallized from alcohol. 7.1 g of product is obtained, corresponding to 61% of the theory. The melting point is 91° C.

후처리

  1. customAfter the solvent has been removed
  2. customthe residue is recrystallized from alcohol

출처 및 근거

ORD 기록
ord-0fb3f5fddbad49e8bda16a28667d452a
출처 데이터셋
uspto-grants-1980_08
특허 번호
US04218460

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