Water → HCID 13776037、化合物

HRID 845344ノート

反応式

HRID 845344 の反応式
[CH2:1]([CH:13]1[CH2:18][C:17](=O)[CH2:16][CH2:15][C:14]1=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[C:21](#[N:25])[CH2:22][C:23]#[N:24].O>NCCC(O)=O.C(Cl)(Cl)Cl>[C:23]([C:22]([C:21]#[N:25])=[C:14]1[CH2:15][CH2:16][C:17](=[C:22]([C:21]#[N:25])[C:23]#[N:24])[CH2:18][CH:13]1[CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])#[N:24]

参加物

6

反応物 3

HCID 962WaterHCID 8010MalononitrileHCID 137760342-Dodecylcyclohexane-1,4-dione

生成物 1

HCID 13776037HCID 13776037、化合物

試薬・触媒・溶媒 2

HCID 239Beta-Alanine触媒HCID 6212Chloroform溶媒

実験手順

A mixture of 2 g (0.0071M) of thus obtained 2-dodecyl-1,4-cyclohexane-dione and 1.4 g (0.0212M) of malononitrile was heated in a water bath to make a solution. β-alanine as a catalyst and 2 ml of water were added to the solution and stirred at a temperature between 40° C. and 50° C. for 8 hours to react the mixture. After cooling, the reacted mixture was dissolved in chloroform, and rinsed with water and dried. The dried material was concentrated under reduced pressure, and purified through silica gel column chromatography. As a result, 1.26 g of white crystal of 1,4-bis-(dicyanomethylene)-2-dodecyl cyclohexane was obtained. The obtained compound had a melting point of 97° C. and an infrared absorption band of 2250 cm-1 which corresponds to a cyano group.

後処理

  1. temperaturewas heated in a water bath
  2. customto react the mixture
  3. temperatureAfter cooling
  4. washrinsed with water
  5. customdried
  6. concentrationThe dried material was concentrated under reduced pressure
  7. custompurified through silica gel column chromatography

出典と根拠

ORDレコード
ord-e50fbc96f6d446cbbb52ea8bd566fba3
出典データセット
uspto-grants-1988_07
特許番号
US04758381

反応ノート

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