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Formaldehyde → 1-[4-(p-Fluorophenyl)-4-hydroxy-2-butynyl]-4-(p-chlorophenyl)-4-hydroxypiperidine

HRID 596947
ノート
印刷プレビュー

反応式

HRID 596947 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([OH:14])[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[CH2:15]=O.[F:17][C:18]1[CH:23]=[CH:22][C:21]([CH:24]([OH:27])[C:25]#[CH:26])=[CH:20][CH:19]=1>O1CCOCC1.O>[F:17][C:18]1[CH:19]=[CH:20][C:21]([CH:24]([OH:27])[C:25]#[C:26][CH2:15][N:11]2[CH2:10][CH2:9][C:8]([C:5]3[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=3)([OH:14])[CH2:13][CH2:12]2)=[CH:22][CH:23]=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

6

反応物 3

HCID 712FormaldehydeHCID 382824-(4-Chlorophenyl)-4-hydroxypiperidineHCID 112751051-(4-Fluorophenyl)prop-2-yn-1-ol

生成物 1

HCID 132773661-[4-(p-Fluorophenyl)-4-hydroxy-2-butynyl]-4-(p-chlorophenyl)-4-hydroxypiperidine収率 77%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回
HCID 31275
1,4-Dioxane
溶媒
2 回

反応条件

温度
80 °C

実験手順

To a solution of 4-(p-chlorophenyl)-4-hydroxypiperidine (4.00 g) in a mixture of dioxane (30 ml), water (10 ml), and 37 % formalin (2.06 g), there were added a solution of 3-(p-fluorophenyl)-3-hydroxy-1-propyne (2.38 g) in dioxane (5 ml) and a solution of cupric sulfate pentahydrate (127 mg) in water (4 ml) under ice-cooling. The resulting mixture was heated at 80° C for 2 hours and, after cooling, the resulting mixture was filtered and the filtrate was concentrated under reduced pressure and extracted with chloroform. The chloroform extracts were dried over magnesium sulfate. After evaporation of the solvent, the residual oil was chromatographed on silica gel to afford 1-[4-(p-fluorophenyl)-4-hydroxy-2-butynyl]-4-(p-chlorophenyl)-4-hydroxypiperidine (4.56 g) as white crystals, M.P. 145° - 146.2° C.

後処理

  1. temperatureafter cooling
  2. filtrationthe resulting mixture was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. extractionextracted with chloroform
  5. dry with materialThe chloroform extracts were dried over magnesium sulfate
  6. customAfter evaporation of the solvent
  7. customthe residual oil was chromatographed on silica gel

出典と根拠

ORDレコード
ord-47faf86cc8014f3d8c710ff54681a8c2
出典データセット
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04012515

反応ノート

読み込み中…

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