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1H-1,2,4-Triazole → 2-chloro-2',6'-dimethyl-N-(1,2,4-triazol-1-yl-methyl)-acetanilide

HRID 1981601
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HRID 1981601 반응식
[Cl:1][CH2:2][C:3]([N:5]([CH2:14]Cl)[C:6]1[C:11]([CH3:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH3:13])=[O:4].[NH:16]1[CH:20]=[N:19][CH:18]=[N:17]1>O1CCCC1>[Cl:1][CH2:2][C:3]([N:5]([CH2:14][N:16]1[CH:20]=[N:19][CH:18]=[N:17]1)[C:6]1[C:11]([CH3:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH3:13])=[O:4]
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참가 물질

4

반응물 2

HCID 92571H-1,2,4-TriazoleHCID 130698822-Chloro-N-(chloromethyl)-N-(2,6-dimethylphenyl)acetamide

생성물 1

HCID 130141982-chloro-2',6'-dimethyl-N-(1,2,4-triazol-1-yl-methyl)-acetanilide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

16.5 parts by weight of 2-chloro-2',6'-dimethyl-N-chloromethyl acetanilide and 9.3 parts by weight of 1,2,4-triazole are refluxed for 8 hours in 60 parts by volume of anhydrous tetrahydrofuran. After the mixture has been cooled, it is filtered, the filtrate is concentrated in vacuo, and the residue is dissolved in 60 parts by volume of chloroform, washed 3 times with water, each time with 40 parts by volume, and dried over sodium sulfate. After evaporation of the solvent in vacuo, there is isolated 21.0 parts by weight of 2-chloro-2',6'-dimethyl-N-(1,2,4-triazol-1-yl-methyl)-acetanilide, m.p.: 115°-118° C.; after recrystallization from ethanol, it melts at 120° C.

후처리

  1. temperatureAfter the mixture has been cooled
  2. filtrationit is filtered
  3. concentrationthe filtrate is concentrated in vacuo
  4. dissolutionthe residue is dissolved in 60 parts by volume of chloroform
  5. washwashed 3 times with water
  6. dry with materialeach time with 40 parts by volume, and dried over sodium sulfate
  7. customAfter evaporation of the solvent in vacuo

출처 및 근거

ORD 기록
ord-9d8613d64975456d8a66653c3a20dfcf
출처 데이터셋
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04593104

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