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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
ノート
印刷プレビュー

反応式

HRID 1981601 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9d8613d64975456d8a66653c3a20dfcf
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04593104

反応ノート

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