Tetrahydrofuran → HCID 53986092、化合物

HRID 1599991ノート

反応式

HRID 1599991 の反応式
[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]

参加物

4

反応物 3

HCID 8028TetrahydrofuranHCID 12295222Cyanamide, 2-propenyl-HCID 53725594HCID 53725594、化合物

生成物 1

HCID 53986092HCID 53986092、化合物

反応条件

温度
55 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-91bc213efd4b4ce8b0f2c6135cf38971
出典データセット
uspto-grants-1998_04
特許番号
US05744426

反応ノート

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