Methane → Benzenamine, 3-chloro-2,6-dinitro-N,N-dipropyl-4-(trifluoromethyl)-

HRID 1658946ノート

反応式

HRID 1658946 の反応式
[Cl:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6](Cl)[C:5]([N+:12]([O-:14])=[O:13])=[CH:4][C:3]=1[C:15]([F:18])([F:17])[F:16].[CH2:19]([NH:22][CH2:23][CH2:24][CH3:25])[CH2:20][CH3:21].C>C(O)C>[CH2:19]([N:22]([CH2:23][CH2:24][CH3:25])[C:6]1[C:5]([N+:12]([O-:14])=[O:13])=[CH:4][C:3]([C:15]([F:18])([F:17])[F:16])=[C:2]([Cl:1])[C:7]=1[N+:8]([O-:10])=[O:9])[CH2:20][CH3:21]

参加物

5

反応物 3

HCID 297MethaneHCID 8902DipropylamineHCID 943982,4-Dichloro-1,3-dinitro-5-(trifluoromethyl)benzene

生成物 1

HCID 94399Benzenamine, 3-chloro-2,6-dinitro-N,N-dipropyl-4-(trifluoromethyl)-収率 79.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A heavy walled glass reaction tube of approximately 50 ml. capacity was charged with 7.0 grams (0.023 mole) of 2,4-dichloro-3,5-dinitrobenzotrifluoride, 4.64 grams (0.0458 mole) of di-n-propylamine and 40 ml. of absolute ethanol. The tube was sealed and heated in an oil bath at 94°-99°C. for 98 hours. The cooled reaction mixture was then evaporated to dryness to give an oily residue which was extracted with boiling diethyl ether. The insoluble di-n-propylamine hydrochloride was removed by filtration and washed with additional ether. The combined ether filtrates were evaporated to give an oily orange residue which was dissolved in 100 ml. of absolute ethanol and decolorized with activated charcoal. The ethanol and volatiles were removed by evaporation under reduced pressure to give the product (6.77 grams) as a viscous reddish oil.

後処理

  1. customA heavy walled glass reaction tube of approximately 50 ml
  2. customThe tube was sealed
  3. temperatureheated in an oil bath at 94°-99°C. for 98 hours
  4. customThe cooled reaction mixture
  5. customwas then evaporated to dryness
  6. customto give an oily residue which
  7. extractionwas extracted with boiling diethyl ether
  8. customThe insoluble di-n-propylamine hydrochloride was removed by filtration
  9. washwashed with additional ether
  10. customThe combined ether filtrates were evaporated
  11. customto give an oily orange residue which
  12. dissolutionwas dissolved in 100 ml
  13. customThe ethanol and volatiles were removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-cb7ca2022d994848beb0fefa0503376b
出典データセット
uspto-grants-1976_06
特許番号
US03966816

反応ノート

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