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

HRID 2210977
ノート
印刷プレビュー

反応式

HRID 2210977 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6342
Acetonitrile
溶媒

反応条件

温度
10 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-dd57b33b8a404a48bde8f61a830e18f5
出典データセット
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05461153

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート