Triethylamine → 4-Methyl-5-trifluoromethyl-3-(1,2-dichloro-2-cyanovinyl thio)-1,2,4-triazole

HRID 1632728ノート

反応式

HRID 1632728 の反応式
[SH:1][C:2]1[N:6]([CH3:7])[C:5]([C:8]([F:11])([F:10])[F:9])=[N:4][N:3]=1.[Cl:12][C:13](Cl)=[C:14]([Cl:17])[C:15]#[N:16].C(N(CC)CC)C>C(Cl)Cl>[CH3:7][N:6]1[C:5]([C:8]([F:9])([F:11])[F:10])=[N:4][N:3]=[C:2]1[S:1][C:13]([Cl:12])=[C:14]([Cl:17])[C:15]#[N:16]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 853312,3,3-Trichloro-2-propenenitrileHCID 178481704HCID 178481704、化合物2 回

生成物 1

HCID 545611114-Methyl-5-trifluoromethyl-3-(1,2-dichloro-2-cyanovinyl thio)-1,2,4-triazole収率 25.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred mixture of 3.5 g (0.0192 mole) 3-mercapto-4-methyl-5-trifluoromethyl-1,2,4-triazole (the product of Example 6) and 3.0 g (0.0192 mole) trichloro-acrylonitrile in methylene chloride, 1.94 g (0.0192 mole) triethylamine in methylene chloride were added dropwise. The reaction mixture was stirred at room temperature for several days. The reaction mixture was washed with water and then dried over magnesium sulfate. The organic phase was passed through a short silica gel (SiO2) column and stripped to give a thick oil which soon crystallized. The material was recrystallized from methylene chloride/hexane to give 1.5 g of the above-identified product as a light yellow solid, melting point 90°-94° C.

後処理

  1. additionwere added dropwise
  2. washThe reaction mixture was washed with water
  3. dry with materialdried over magnesium sulfate
  4. customto give a thick oil which
  5. customsoon crystallized
  6. customThe material was recrystallized from methylene chloride/hexane

出典と根拠

ORDレコード
ord-4ccf332290194fc8a958458b6d2ed95b
出典データセット
uspto-grants-1984_10
特許番号
US04477459

反応ノート

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