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

HRID 1632728노트

반응식

HRID 1632728 반응식
[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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 853312,3,3-Trichloro-2-propenenitrileHCID 178481704HCID 178481704, 화합물2회

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4ccf332290194fc8a958458b6d2ed95b
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04477459

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