(Aminomethyl)phosphonic acid → HCID 22132222、化合物

HRID 618645

反応式

HRID 618645 の反応式
[NH2:1][CH2:2][P:3]([OH:6])(=[O:5])[OH:4].[F:7][C:8]([F:21])([F:20])[C:9]1[CH:10]=[C:11]([N+:17]([O-:19])=[O:18])[C:12](Cl)=[CH:13][C:14]=1[Cl:15]>O.C(O)C>[N+:17]([C:11]1[CH:10]=[C:9]([C:8]([F:7])([F:20])[F:21])[C:14]([Cl:15])=[CH:13][C:12]=1[NH:1][CH2:2][P:3]([OH:6])(=[O:4])[OH:5])([O-:19])=[O:18]

参加物

5

反応物 2

HCID 14017(Aminomethyl)phosphonic acidHCID 6211792,4-Dichloro-5-nitrobenzotrifluoride

生成物 1

HCID 22132222HCID 22132222、化合物収率 68.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

3.3 g (30 mmol) of aminomethanephosphonic acid in 120 ml of water and 120 ml of ethanol are introduced together with 3.37 g (31.8 mmol) of soda and mixed with 7.8 g (97%, 30 mmol) of 3-trifluoromethyl-4,6-dichloronitrobenzene, and it is refluxed for 4 hours at 120° C. bath temperature. After removing the ethanol in a rotary evaporator, it is extracted three times with 100 ml of ethyl acetate. The organic phase is washed with a little water. It contains starting material and is discarded. The collected aqueous phase is adjusted acidic with 4 N hydrochloric acid to pH 1 and extracted three times with 100 ml of ethyl acetate each. The organic phase is washed with water, dried, filtered and concentrated by evaporation. 6.85 g (68% of theory) of N-(2-nitro-4-trifluoromethyl-5-chloro-phenyl)-aminomethanephosphonic acid of melting point 207.3° C. is obtained.

後処理

  1. customAfter removing the ethanol
  2. customin a rotary evaporator, it
  3. extractionis extracted three times with 100 ml of ethyl acetate
  4. washThe organic phase is washed with a little water
  5. extractionextracted three times with 100 ml of ethyl acetate each
  6. washThe organic phase is washed with water
  7. customdried
  8. filtrationfiltered
  9. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-59297c84265743d68a9221d0db48b81b
出典データセット
uspto-grants-1999_09
特許番号
US05955461

関連ノート

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