Acetic Acid → 2-(((1,1,1-Trifluoro-2-methylpropan-2-yl)amino)methylene)-succinonitrile

HRID 624656

반응식

HRID 624656 반응식
[CH:1](OCC)=O.[C:6](#[N:11])[CH2:7][CH2:8][C:9]#[N:10].C[O-].[Na+].[F:15][C:16]([F:22])([F:21])[C:17]([CH3:20])([NH2:19])[CH3:18].C(O)(=O)C>C1(C)C=CC=CC=1>[F:15][C:16]([F:22])([F:21])[C:17]([NH:19][CH:1]=[C:8]([CH2:7][C:6]#[N:11])[C:9]#[N:10])([CH3:20])[CH3:18]

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 8025Ethyl formateHCID 8062SuccinonitrileHCID 10942334Sodium MethoxideHCID 112751881,1,1-Trifluoro-2-methylpropan-2-amine

생성물 1

HCID 900230042-(((1,1,1-Trifluoro-2-methylpropan-2-yl)amino)methylene)-succinonitrile

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

A solution of ethyl formate (330 mg, 4.46 mmol) and succinonitrile (300 mg, 3.75 mmol) in toluene (1561 μl) was added dropwise to a suspension of sodium methanolate (215 mg, 3.97 mmol) in toluene (1561 μl) at 0° C. After being stirred at RT for 3 h, the reaction mixture was treated with 1,1,1-trifluoro-2-methylpropan-2-amine (486 mg, 3.82 mmol) and acetic acid (255 μl, 4.46 mmol) then heated at 120° C. for 3 h. After being cooled to RT, the reaction mixture was washed with brine, then dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to afford the title compound as a brown oil, which was used without further purification.

후처리

  1. temperaturethen heated at 120° C. for 3 h
  2. temperatureAfter being cooled to RT
  3. washthe reaction mixture was washed with brine
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6830fa9bd52c4e4f868e2f2c20af2d0b
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09303045B2

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