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Pentafluoropyridine → Imidazole

HRID 379612
ノート
印刷プレビュー

反応式

HRID 379612 の反応式
[Li]CCCC.C(OC([N:13]1[C:17]([C:18]2[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=2)=[C:16]([C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=2)[N:15]=[CH:14]1)OCC)C.C(OC([N:38]1[C:42](C2C=CC(F)=CC=2)=[C:41](C2C=CN=CC=2)[N:40]=[CH:39]1)OCC)C.[F:56][C:57]1[N:62]=[C:61]([F:63])[C:60]([F:64])=[C:59](F)[C:58]=1[F:66]>C1COCC1>[F:30][C:27]1[CH:26]=[CH:25][C:24]([C:16]2[N:15]=[C:14]([C:59]3[C:58]([F:66])=[C:57]([F:56])[N:62]=[C:61]([F:63])[C:60]=3[F:64])[NH:13][C:17]=2[C:18]2[CH:19]=[CH:20][N:21]=[CH:22][CH:23]=2)=[CH:29][CH:28]=1.[NH:38]1[CH:42]=[CH:41][N:40]=[CH:39]1
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 69690PentafluoropyridineHCID 183675041-(1,1-Diethoxymethyl)-4-(4-fluorophenyl)-5-(4-pyridinyl)imidazoleHCID 183675051-(1,1-Diethoxymethyl)-5-(4-fluorophenyl)-4-(4-pyridinyl)imidazoleHCID 178418339Butyllithium

生成物 2

HCID 795ImidazoleHCID 20692711
2,3,5,6-Tetrafluoro-4-[4-(4-fluoro-phenyl)-5-pyridin-4-yl-1H-imidazol-2-yl]-pyridine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-55 °C

実験手順

1.6 M nBuLi (66 ml; 45 mmol) is added at −45° C. to a ˜1:1 mixture of 1-(1,1-diethoxymethyl)-4-(4-fluorophenyl)-5-(4-pyridinyl)imidazole and 1-(1,1-diethoxymethyl)-5-(4-fluorophenyl)-4-(4-pyridinyl)imidazole (15 g; 43 mmol) in THF (210 ml). After 15 min. at −45° C. the reaction mixture is cooled to −55° C. and pentafluoropyridine (5.1 ml; 47 mmol) is rapidly introduced. The cooling bath is removed, the reaction mixture allowed to warm to −15° C. and poured on water (1 l), which is then acidified with 2N HCl (100 ml). After stirring for 5 min. the mixture is combined with a saturated solution of Na2CO3 and extracted with ethyl acetate three times. The combined organic phases are dried over Na2SO4, filtered and evaporated to dryness rendering the title compound as brownish crystals (16.3 g). Chromatography (SiO2; acetone/hexanes 1:1) yields the title compound together with some unreacted and unprotected imidazole starting material, which could be removed by washing with acetone yielding the title compound (8.7 g; 52.4%).

後処理

  1. customThe cooling bath is removed
  2. temperatureto warm to −15° C.
  3. additionpoured on water (1 l), which
  4. extractionextracted with ethyl acetate three times
  5. dry with materialThe combined organic phases are dried over Na2SO4
  6. filtrationfiltered
  7. customevaporated to dryness rendering the title compound as brownish crystals (16.3 g)

出典と根拠

ORDレコード
ord-b44df5b3ba744d918c9a74fa57fc2599
出典データセット
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06300347B1

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