Toluene → HCID 13650461、化合物

HRID 1165488ノート

反応式

HRID 1165488 の反応式
[N:1]1([CH2:6][C:7]([C:9]2[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=2)=[O:8])[CH:5]=[N:4][CH:3]=[N:2]1.O[CH2:17][N:18]1[CH:22]=[N:21][CH:20]=[N:19]1.C1(C)C=CC=CC=1.N1CCCCC1>O.C(O)(=O)C>[Cl:15][C:12]1[CH:13]=[CH:14][C:9]([C:7](=[O:8])[CH:6]([N:1]2[CH:5]=[N:4][CH:3]=[N:2]2)[CH2:17][N:18]2[CH:22]=[N:21][CH:20]=[N:19]2)=[CH:10][CH:11]=1

参加物

7

反応物 4

HCID 1140TolueneHCID 8082PiperidineHCID 7164721-(4-Chlorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethan-1-oneHCID 1547783(1H-1,2,4-Triazol-1-yl)methanol

生成物 1

HCID 13650461HCID 13650461、化合物収率 78.5%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

A mixture of 44.3 g of 4-chlorophenyl 1,2,4-triazol-1-ylmethyl ketone, 19.6 g of 1-hydroxymethyl-1,2,4-triazole, 300 ml of toluene, 6 g of acetic acid and 2 ml of piperidine is heated under a water separator until separation of water is complete. The mixture is allowed to cool, and the resulting crystalline precipitate is filtered off with suction and washed with diisopropyl ether. 47 g (76% of theory) of 1-(4-chlorophenyl)-2,3-di(1,2,4-triazol-1-yl)-1-propanone of melting point 204° C., are obtained.

後処理

  1. temperatureto cool
  2. filtrationthe resulting crystalline precipitate is filtered off with suction
  3. washwashed with diisopropyl ether

出典と根拠

ORDレコード
ord-06a1928773e5470393aa4949f397a73a
出典データセット
uspto-grants-1990_03
特許番号
US04910213

反応ノート

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