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Sec-Butylamine → 3-Chloro-N-(1-methylpropyl)-2,4-dinitro-6-(trifluoromethyl)benzenamine

HRID 1658947
ノート
印刷プレビュー

反応式

HRID 1658947 の反応式
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([Cl:11])[C:5]([N+:12]([O-:14])=[O:13])=[CH:4][C:3]=1[C:15]([F:18])([F:17])[F:16].[CH:19]([NH2:23])([CH2:21][CH3:22])[CH3:20]>C(O)C>[CH:19]([NH:23][C:2]1[C:3]([C:15]([F:18])([F:17])[F:16])=[CH:4][C:5]([N+:12]([O-:14])=[O:13])=[C:6]([Cl:11])[C:7]=1[N+:8]([O-:10])=[O:9])([CH2:21][CH3:22])[CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24874Sec-ButylamineHCID 943982,4-Dichloro-1,3-dinitro-5-(trifluoromethyl)benzene

生成物 1

HCID 214130983-Chloro-N-(1-methylpropyl)-2,4-dinitro-6-(trifluoromethyl)benzenamine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred mixture of 20 g. (0.0655 mole) of 2,4-dichloro-3,5-dinitrobenzotrifluoride and 150 ml. of absolute ethanol was added 9.58 g. (0.131 mole) of sec-butylamine, dropwise, over a period of about 15 minutes. The resultant solution was refluxed for two hours and the ethanol then removed by distillation under reduced pressure. The solid yellow residue was triturated with 300 ml. water to dissolve the sec-butylamine hydrochloride. The water insoluble product was isolated by filtration, washed with water, and then dissolved in 600 ml. of refluxing 95% ethanol. Upon cooling, the product crystallized. Filtration gave 20.4 g. of a yellow crystalline solid, melting at 90.5° - 91.5°C.

後処理

  1. additionTo a stirred mixture of 20 g
  2. customthe ethanol then removed by distillation under reduced pressure
  3. customThe solid yellow residue was triturated with 300 ml
  4. dissolutionwater to dissolve the sec-butylamine hydrochloride
  5. customThe water insoluble product was isolated by filtration
  6. washwashed with water
  7. dissolutiondissolved in 600 ml
  8. temperatureof refluxing 95% ethanol
  9. temperatureUpon cooling
  10. customthe product crystallized
  11. filtrationFiltration
  12. customgave 20.4 g

出典と根拠

ORDレコード
ord-413a1681bb004f1a9fd2c7458fb1b079
出典データセット
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03966816

反応ノート

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