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Diethylamine → HCID 13385730, 화합물

HRID 1731955
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HRID 1731955 반응식
Cl[C:2]1[C:3]2[N:4]([C:12]([C:15]([F:18])([F:17])[F:16])=[N:13][N:14]=2)[C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.[CH2:19]([NH:21][CH2:22][CH3:23])[CH3:20]>CN(C)C=O>[CH2:19]([N:21]([CH2:22][CH3:23])[C:2]1[C:3]2[N:4]([C:12]([C:15]([F:18])([F:17])[F:16])=[N:13][N:14]=2)[C:5]2[C:10]([N:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8021DiethylamineHCID 14280609HCID 14280609, 화합물

생성물 1

HCID 13385730HCID 13385730, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture consisting of 700 mg. (0.0025 mole) of 4-chloro-1-trifluoromethyl-[1,2,4]triazolo[4,3-a]quinoxaline (prepared as described above) and 560 mg. (0.0075 mole) of diethylamine (0.8 ml.) in 10 ml. of N,N-dimethylformamide was stirred at room temperature overnight and then poured over ice. The resulting mixture was then filtered and the recovered solid product washed with water and then dissolved in ethyl acetate. The latter organic solution was next washed with saturated brine and dried over anhydrous magnesium sulfate. After removal of the drying agent by means of filtration and the solvent by means of evaporation under reduced pressure, there are ultimately obtained a light yellow solid which after recrystallization from diethyl ether gave pure 4-diethylamino-1-trifluoromethyl-[1,2,4]triazolo[4,3-a]quinoxaline. The yield of the first crop melting at 155°-157° C. amounted to 260 mg. (34%), while the yield of the second crop melting at 153°-156° C. amounted to 170 mg. (22%).

후처리

  1. additionpoured over ice
  2. filtrationThe resulting mixture was then filtered
  3. washthe recovered solid product washed with water
  4. dissolutiondissolved in ethyl acetate
  5. washnext washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customAfter removal of the drying agent
  8. filtrationby means of filtration
  9. customthe solvent by means of evaporation under reduced pressure, there
  10. customare ultimately obtained a light yellow solid which
  11. customafter recrystallization from diethyl ether

출처 및 근거

ORD 기록
ord-c59ff791f0ab4d6e87d83583c6cbf37d
출처 데이터셋
uspto-grants-1986_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04623725

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