Tert-Butyl nitrite → HCID 14651251, 화합물

HRID 232648노트

반응식

HRID 232648 반응식
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]

참가 물질

4

반응물 2

HCID 10906Tert-Butyl nitriteHCID 23359007HCID 23359007, 화합물

생성물 1

HCID 14651251HCID 14651251, 화합물수율 49%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ebcf91937c4246739a04427c37bb4391
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591744

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