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Carbon Dioxide → HCID 54085765、化合物

HRID 126843
ノート
印刷プレビュー

反応式

HRID 126843 の反応式
[N:1]1([CH2:7][CH:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[C:14]([CH2:16][C:17](O)=O)#[N:15].C=O.[C:22](=O)=O>CCOCC.O1CCOCC1>[N:1]1([CH2:7][CH:8]2[CH2:9][CH2:10][N:11]([CH2:22][C:16](=[CH2:17])[C:14]#[N:15])[CH2:12][CH2:13]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]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 280Carbon DioxideHCID 712FormaldehydeHCID 9740Cyanoacetic acidHCID 128029051-(Piperidin-4-ylmethyl)piperidine

生成物 1

HCID 54085765HCID 54085765、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒
HCID 31275
1,4-Dioxane
溶媒

反応条件

温度
22 °C

実験手順

4-(1-Piperidylmethyl)piperidine (0.05 mole) was dissolved in 17 ml. of dioxane containing cyanoacetic acid (4.25 g., 0.05 mole) by warming and the solution then cooled to 22° C. Over a 9 minute period, 37% aqueous formaldehyde (8.5 g., 0.1 mole) was dripped in. The temperature throughout the addition was 25°-28° C. It was then warmed to 35°-40° C. for carbon dioxide evolution and maintained then for 2 hours. The mixture was stripped at a bath temperature of 60° C./15 mm. to leave approximately 12 g. of an oil. Most dissolved in 150 ml. of ether; the solution was washed twice with water, dried over anhydrous sodium sulfate and the solvent stripped. A nearly colorless oil was obtained, 8.6 g., which gradually solidified on standing at room temperature.

後処理

  1. temperatureby warming
  2. additionThe temperature throughout the addition
  3. customwas 25°-28° C
  4. temperaturemaintained
  5. customThe mixture was stripped at a bath
  6. customtemperature of 60° C./15 mm
  7. customto leave approximately 12 g
  8. dissolutionMost dissolved in 150 ml
  9. washthe solution was washed twice with water
  10. dry with materialdried over anhydrous sodium sulfate
  11. customA nearly colorless oil was obtained
  12. customon standing at room temperature

出典と根拠

ORDレコード
ord-e28685f225704fc79f7b328e61926364
出典データセット
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04254131

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