Tetrahydrofuran → HCID 53986092, 화합물

HRID 1599991노트

반응식

HRID 1599991 반응식
[CH2:1]([NH:4][C:5]#[N:6])[CH:2]=[CH2:3].[Cl:7][C:8](=[CH:12][C:13]1[CH:18]=[C:17]([C:19]2[C:23]([Cl:24])=[C:22]([O:25][CH:26]([F:28])[F:27])[N:21]([CH3:29])[N:20]=2)[C:16]([Cl:30])=[CH:15][C:14]=1[Cl:31])[C:9](Cl)=[O:10].[O:32]1CCCC1>>[CH2:1]([N:4]([C:5]([NH2:6])=[O:32])[C:9](=[O:10])[C:8]([Cl:7])=[CH:12][C:13]1[CH:18]=[C:17]([C:19]2[C:23]([Cl:24])=[C:22]([O:25][CH:26]([F:28])[F:27])[N:21]([CH3:29])[N:20]=2)[C:16]([Cl:30])=[CH:15][C:14]=1[Cl:31])[CH:2]=[CH2:3]

참가 물질

4

반응물 3

HCID 8028TetrahydrofuranHCID 12295222Cyanamide, 2-propenyl-HCID 53725594HCID 53725594, 화합물

생성물 1

HCID 53986092HCID 53986092, 화합물

반응 조건

온도
55 °C

실험 절차

0.36 g (4.4 mmol) of allylcyanamide were added to a suspension of 2 g (4.4 mmol) of 2-chloro-3-(2,4-dichloro-5-(4-chloro-5-difluoromethoxy-1-methyl-1H-pyrazol-3-yl)phenyl)Propenoyl chloride and 0.8 g (5.8 mmol) of potassium carbonate(ground) in 50 ml of tetrahydrofuran. The reaction mixture was stirred at 50 to 60° C. for 5 hours and then concentrated. The residue was taken up in ethyl acetate, after which the organic phase was washed with water, dried over magnesium sulfate and concentrated. The crude product was purified by means of column chromatography on silica gel (eluent: ethyl acetate) followed by crystallization from diisopropyl ether. Yield: 0.2 g.

후처리

  1. concentrationconcentrated
  2. washafter which the organic phase was washed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe crude product was purified by means of column chromatography on silica gel (eluent: ethyl acetate)
  6. customfollowed by crystallization from diisopropyl ether

출처 및 근거

ORD 기록
ord-91bc213efd4b4ce8b0f2c6135cf38971
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05744426

반응 노트

불러오는 중…