Ammonium Chloride → HCID 68320915, 화합물

HRID 2047467노트

반응식

HRID 2047467 반응식
Cl.[CH3:2][C:3]1[CH:4]=[C:5]([CH:7]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:9]=1)[NH2:6].[C:14](Cl)(=[O:25])[O:15][C:16]1[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][CH:17]=1.C(N(CC)C(C)C)(C)C.[Cl-].[NH4+]>C1COCC1>[CH3:2][C:3]1[CH:4]=[C:5]([NH:6][C:14](=[O:25])[O:15][C:16]2[CH:17]=[CH:18][C:19]([N+:22]([O-:24])=[O:23])=[CH:20][CH:21]=2)[CH:7]=[C:8]([C:10]([F:11])([F:12])[F:13])[CH:9]=1

참가 물질

6

반응물 4

HCID 25517Ammonium ChlorideHCID 81531DiisopropylethylamineHCID 821294-Nitrophenyl chloroformateHCID 866556663-Methyl-5-(trifluoromethyl)aniline hydrochloride

생성물 1

HCID 68320915HCID 68320915, 화합물수율 98.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
5 °C

실험 절차

3-Methyl-5-(trifluoromethyl)aniline monohydrochloride (2.93 g) synthesized in reference to a known method (U.S. Pat. No. 4,532,353) was dissolved in THF (25 mL), and 4-nitrophenyl chlorocarbonate (3.07 g) and N,N-diisopropylethylamine (1.97 mL) were added dropwise at 5° C. The reaction mixture was stirred at 5° C. for 1 hr, poured into saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried and concentrated under reduced pressure to give the title compound (4.66 g) as a white powder.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with water and saturated brine
  3. customdried
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-567a16b07d4f48649a629d309bec7986
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08592454B2

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