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Ethyl Acetate → HCID 18951395、化合物

HRID 1492720
ノート
印刷プレビュー

反応式

HRID 1492720 の反応式
C(N(CC)CC)C.[CH3:8][C:9]1[C:14]([S:15]([OH:18])(=[O:17])=[O:16])=[CH:13][CH:12]=[C:11]([CH3:19])[N:10]=1.[F:20]F.C(OCC)(=O)C>C(#N)C>[F:20][N+:10]1[C:11]([CH3:19])=[CH:12][CH:13]=[C:14]([S:15]([O-:18])(=[O:17])=[O:16])[C:9]=1[CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 24524Fluorine2 回HCID 86748337HCID 86748337、化合物

生成物 1

HCID 18951395HCID 18951395、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a mixture of acetonitrile (4 ml) and 2,6-dimethylpyridine-3-sulfonic acid (410 mg, 2 mmol), triethylamine (404 mg, 4 mmol) was added at room temperature while stirring, followed by evaporation to dryness under reduced pressure to obtain 2,6-dimethylpyridine-3-sulfonic acid triethylamine salt. The triethylamine salt was dissolved in acetonitrile (4 ml). To the resulting solution cooled with a cooling bath kept at -20° C., a mixed gas of 10% fluorine/ 90% nitrogen was introduced at a flow rate of 15 ml/min. The total amount of the fluorine gas was 6 mmol. Thereafter, the nitrogen gas alone was introduced for 30 minutes. Ethyl acetate was added to the reaction mixture. The precipitated crystal was recovered by filtration to obtain N-fluoro-2,6-dimethylpyridinium-3-sulfonate (257 mg). Yield, 63%. Decomposition point, 200°-210° C.

後処理

  1. temperatureTo the resulting solution cooled with a cooling bath
  2. customkept at -20° C.
  3. additionThereafter, the nitrogen gas alone was introduced for 30 minutes
  4. filtrationThe precipitated crystal was recovered by filtration

出典と根拠

ORDレコード
ord-d6c271d2975a4cb1b872ce8a4b196c8b
出典データセット
uspto-grants-1994_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05374732

反応ノート

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