Trifluoroacetonitrile → HCID 178458719, 화합물

HRID 2073688

반응식

HRID 2073688 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][CH:10]([CH3:12])[CH3:11])=[CH:4][C:3]=1[NH:13][NH2:14].[F:15][C:16]([F:20])([F:19])[C:17]#[N:18]>CO.CCCCC>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9][CH:10]([CH3:12])[CH3:11])=[CH:4][C:3]=1[NH:13][NH:14][C:17](=[NH:18])[C:16]([F:20])([F:19])[F:15]

참가 물질

5

반응물 2

HCID 67710TrifluoroacetonitrileHCID 170281(2,4-Dichloro-5-(1-methylethoxy)phenyl)hydrazine

생성물 1

HCID 178458719HCID 178458719, 화합물수율 87.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8003Pentane용매

실험 절차

Under a dry nitrogen atmosphere a stirred solution of 2.4 g (0.01 mole) of 2,4-dichloro-5-(1-methylethoxy)phenylhydrazine in 140 mL of methanol was cooled to -60° C. in a dry ice-isopropanol bath. Trifluoroacetonitrile (23.2 g, 0.24 mole) was bubbled into the cold solution during a two minute period. After complete addition the cold solution was stirred for 30 minutes, then allowed to warm slowly to room temperature during the next three hours. A stream of nitrogen gas was bubbled into the room temperature solution to aid in the vaporization and removal of trifluoroacetonitrile, leaving a liquid residue. This residue was evaporated further under reduced pressure to leave a resinous material. This material was stirred in cold pentane to produce a solid. The pentane was decanted and the solid triturated in fresh cold pentane. The pentane was decanted and the solid dried under reduced pressure to yield 2.9 g of N-[2,4-dichloro-5-(1-methylethoxy)anilino]trifluoroacetamidine (mp 80.5°-81° C.).

후처리

  1. additionAfter complete addition the cold solution
  2. customA stream of nitrogen gas was bubbled into the room temperature solution to aid in the vaporization and removal of trifluoroacetonitrile
  3. customleaving a liquid residue
  4. customThis residue was evaporated further under reduced pressure
  5. customto leave a resinous material
  6. customto produce a solid
  7. customThe pentane was decanted
  8. customthe solid triturated in fresh cold pentane
  9. customThe pentane was decanted
  10. customthe solid dried under reduced pressure

출처 및 근거

ORD 기록
ord-86946f2bc75e428e93b9c1b86fa90a84
출처 데이터셋
uspto-grants-1990_04
특허 번호
US04919708

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