Ammonia → 3-(2,2-Dichloroethenyl)-2,2-dimethylcyclopropane-1-carbonitrile

HRID 2057513

反応式

HRID 2057513 の反応式
Cl[CH:2]([CH2:12][C:13]([Cl:16])([Cl:15])Cl)[C:3]([CH3:11])([CH3:10])[CH:4]([C:8]#[N:9])C(O)=O.N>CN(C)C=O.O>[Cl:16][C:13]([Cl:15])=[CH:12][CH:2]1[C:3]([CH3:10])([CH3:11])[CH:4]1[C:8]#[N:9]

参加物

5

反応物 2

HCID 222AmmoniaHCID 204348434,6,6,6-Tetrachloro-2-cyano-3,3-dimethylhexanoic acid

生成物 1

HCID 128981733-(2,2-Dichloroethenyl)-2,2-dimethylcyclopropane-1-carbonitrile収率 79%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
140 °C

実験手順

4-Chloro-2-cyano-3,3-dimethyl-6,6,6-trichlorohexanoic acid (40 g) was dissolved in dimethyl formamide (66 ml) and the solution, at room temperature, was saturated with gaseous ammonia with no external cooling. The solution was stirred at 140° C. for 5 hours, then diluted with water and extracted with ether (3×100 ml). The ether solution was washed with saturated NaCl, dried over MgSO4 and evaporated to afford Compound A as a yellow oil (purity 85%) which partly crystallized on standing. Yield 79%.

後処理

  1. customat room temperature
  2. extractionextracted with ether (3×100 ml)
  3. washThe ether solution was washed with saturated NaCl
  4. dry with materialdried over MgSO4
  5. customevaporated

出典と根拠

ORDレコード
ord-bd1e5a5e77bf49c7bc7ba1c55741634c
出典データセット
uspto-grants-1980_07
特許番号
US04211720

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