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Sodium Fluoride → 1-Fluoro-2,4,6-trimethylpyridinium Tetrafluoroborate (Fluorinating Reagent)

HRID 982502
ノート
印刷プレビュー

反応式

HRID 982502 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[N:3]=1.[B-:10]([F:14])([F:13])([F:12])[F:11].[Na+].[F-:16].[Na+].N#N.FF.FF>C(#N)C>[F:11][B-:10]([F:14])([F:13])[F:12].[F:16][N+:3]1[C:4]([CH3:9])=[CH:5][C:6]([CH3:8])=[CH:7][C:2]=1[CH3:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 5235Sodium FluorideHCID 79532,4,6-TrimethylpyridineHCID 24524FluorineHCID 4343483Sodium TetrafluoroborateHCID 131710817Fluorine nitrogen

生成物 1

HCID 27793091-Fluoro-2,4,6-trimethylpyridinium Tetrafluoroborate (Fluorinating Reagent)収率 70%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

In a 25 ml pear-shaped flask, 2,4,6-trimethylpyridine (1.21 g, 10 mmoles), sodium borofluoride (1.23 g, 10 mmoles) as the XM reactant and anhydrous sodium fluoride (2.1 g, 50 mmoles) were dissolved in 15 ml of anhydrous acetonitrile and to the resulting solution a mixed gas of nitrogen/fluorine (9:1) was introduced at a rate of 50 ml/min. at -40° C. under vigorous stirring. The amount of fluorine introduced was 20 mmoles. After the completion of the reaction, precipitates were filtered and then the solvent was distilled off. The resultant residue was recrystallized from acetonitrile/diethyl ether to obtain 1.59 g (yield: 70%) of N-fluoro-2,4,6-trimethylpyridinium tetrafluoroborate the physical properties of which are shown in Table 6.

後処理

  1. additionwas introduced at a rate of 50 ml/min. at -40° C. under vigorous stirring
  2. customAfter the completion of the reaction
  3. customprecipitates
  4. filtrationwere filtered
  5. distillationthe solvent was distilled off
  6. customThe resultant residue was recrystallized from acetonitrile/diethyl ether

出典と根拠

ORDレコード
ord-b91908fd55ed454aaa45f42e0a2abe14
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04996320

反応ノート

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