Triethylamine → HCID 14624371, 화합물

HRID 1650765

반응식

HRID 1650765 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[NH:10][N:11]=[C:12](Br)[C:13]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15].[CH2:21]([N:23]([CH2:26][CH3:27])[C:24]#[N:25])[CH3:22].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH2:21]([N:23]([C:24]1[N:10]([C:3]2[C:2]([Cl:1])=[CH:7][C:6]([Cl:8])=[CH:5][C:4]=2[Cl:9])[N:11]=[C:12]([C:13]([F:19])([F:18])[C:14]([F:17])([F:16])[F:15])[N:25]=1)[CH2:26][CH3:27])[CH3:22]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12050DiethylcyanamideHCID 86743923HCID 86743923, 화합물

생성물 1

HCID 14624371HCID 14624371, 화합물수율 54.3%

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

3.4 g (0.008 mol) of pentafluoropropionyl bromide 2,4,6-trichlorophenylhydrazone and 0.8 g (0.008 mol) of N,N-diethylcyanamide were added to 20 ml of toluene. Then, 0.9 g (0.009 mol) of triethylamine was added thereto under stirring at room temperature. After completion of the dropwise addition, stirring was continued at room temperature for further 1 hour. Then, 20 ml of toluene was added thereto, followed by washing with water. The organic layer was dried, and the solvent was distilled off. The residue was purified by silica gel column chromatography to obtain 1.9 g (yield: 54.3%) of the desired compound as a brown powder. Melting point: 66°-70° C.

후처리

  1. additionAfter completion of the dropwise addition
  2. stirringstirring
  3. washby washing with water
  4. customThe organic layer was dried
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-4dab9342e66f404f853b7217f76fd96a
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04925864

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