Tert-Butyl nitrite → HCID 14651251、化合物

HRID 232648ノート

反応式

HRID 232648 の反応式
N(OC(C)(C)C)=O.[F:8][C:9]1[C:15]([CH3:16])=[C:14]([F:17])[C:13]([F:18])=[C:12]([CH3:19])[C:10]=1N>CN(C)C=O>[F:18][C:13]1[C:14]([F:17])=[C:15]([CH3:16])[C:9]([F:8])=[CH:10][C:12]=1[CH3:19]

参加物

4

反応物 2

HCID 10906Tert-Butyl nitriteHCID 23359007HCID 23359007、化合物

生成物 1

HCID 14651251HCID 14651251、化合物収率 49%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A solution of t-butyl nitrite (4.56 g) in anhydrous dimethylformamide (26.5 ml) is stirred with heating at 50°-52° C. and thereto a solution of 2,4,5-trifluoro-3,6-dimethylaniline (4.24 g) in anhydrous dimethylformamide (40 ml) is added dropwise at 50°-52° C. over a period of 30 minutes. The mixture is further stirred at the same temperature for 30 minutes. After cooling, the mixture is poured into ice-water, extracted with diethyl ether, and the extract is washed with water, and then with diluted hydrochloric acid and dried. The diethyl ether is distilled off under atomospheric pressure and the residue is concentrated and distilled under atomospheric pressure to give 2,3,5-trifluoro-4-methyltoluene (1.9 g), as yellow oil, b.p. 120°-125° C.

後処理

  1. temperaturewith heating at 50°-52° C.
  2. temperatureAfter cooling
  3. extractionextracted with diethyl ether
  4. washthe extract is washed with water
  5. dry with materialwith diluted hydrochloric acid and dried
  6. distillationThe diethyl ether is distilled off under atomospheric pressure
  7. concentrationthe residue is concentrated
  8. distillationdistilled under atomospheric pressure

出典と根拠

ORDレコード
ord-ebcf91937c4246739a04427c37bb4391
出典データセット
uspto-grants-1997_01
特許番号
US05591744

反応ノート

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