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Triethylamine → 2-Ethoxy-4-fluoro-6-hydrazinylpyrimidine

HRID 864626
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HRID 864626 반응식
[CH2:1]([O:3][C:4]1[N:9]=[C:8]([F:10])[CH:7]=[C:6](F)[N:5]=1)[CH3:2].C(N(CC)CC)C.O.[NH2:20][NH2:21].NN>O.C(#N)C>[CH2:1]([O:3][C:4]1[N:9]=[C:8]([F:10])[CH:7]=[C:6]([NH:20][NH2:21])[N:5]=1)[CH3:2]
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참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 9321HydrazineHCID 24654Hydrazine hydrate (1:1)HCID 110409852-Ethoxy-4,6-Difluoropyrimidine

생성물 1

HCID 109429042-Ethoxy-4-fluoro-6-hydrazinylpyrimidine

시약·촉매·용매 2

HCID 962Water용매
HCID 6342
Acetonitrile
용매

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온도
10 °C

실험 절차

A mixture of 100 g of 94 percent purity (0.59 mol) 2-ethoxy-4,6-difluoropyrimidine, 275 mL of acetonitrile, and 107 g of water was prepared and cooled to 10° C. To this was added 68 g (0.67 mol) of triethylamine and then 34 g (0.68 mol) of hydrazine hydrate, slowly with stirring and cooling (at 5° to 10° C). When all of the hydrazine had been added, the mixture was stirred another 15 min with cooling and was then allowed to warm. After a total of 1 hour, the solids that formed were recovered by vacuum filtration and were washed twice with 100 mL portions of water and then with 50 mL of ethanol. The title compound, which was obtained as a white solid melting at 141°-143° C., amounted to 79.7 g (80 percent of theory).

후처리

  1. customwas prepared
  2. temperaturecooling (at 5° to 10° C)
  3. temperaturewith cooling
  4. temperatureto warm
  5. customAfter a total of 1 hour, the solids that formed
  6. filtrationwere recovered by vacuum filtration
  7. washwere washed twice with 100 mL portions of water

출처 및 근거

ORD 기록
ord-cf0fe4eecffe4cad9682fbff2cfe7843
출처 데이터셋
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05563269

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