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Diethyl Malonate → HCID 54455773、化合物

HRID 1388134
ノート
印刷プレビュー

反応式

HRID 1388134 の反応式
[CH2:1]([O:3][C:4](=[O:11])[CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2].CC[O-].[Na+].[Na].[CH:17]1([O:23][CH2:24][CH2:25][CH2:26][CH2:27]Br)[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1>C(O)C>[CH2:1]([O:3][C:4](=[O:11])[CH:5]([CH2:27][CH2:26][CH2:25][CH2:24][O:23][CH:17]1[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]1)[C:6]([O:8][CH2:9][CH3:10])=[O:7])[CH3:2]
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 4

HCID 7761Diethyl MalonateHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 20214109(4-Bromobutoxy)cyclohexane

生成物 1

HCID 54455773HCID 54455773、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

15 g of malonic acid diethyl ester are added dropwise at 50° C. to a solution of sodium ethylate, freshly prepared from 1.5 g of sodium and 30 ml of ethanol. This temperature is maintained for 1 hour and 11.7 g of 4-cyclohexyloxybutyl bromide are then added dropwise. When the addition is complete, the mixture is stirred for 3 hours at 60° C. and is concentrated considerably, 100 ml of ice water are added to the residue and the mixture is extracted 3 times with a total of 150 ml of methylene chloride. The combined organic phases are dried over sodium sulphate and the solvent is removed by distillation in vacuo, together with excess malonic acid diethyl ester. This gives 10.5 g of [4-(cyclohexyloxy)-butyl]-malonic acid diethyl ester in the form of a pale yellow oily residue.

後処理

  1. temperatureThis temperature is maintained for 1 hour
  2. additionWhen the addition
  3. concentrationis concentrated considerably
  4. addition100 ml of ice water are added to the residue
  5. extractionthe mixture is extracted 3 times with a total of 150 ml of methylene chloride
  6. dry with materialThe combined organic phases are dried over sodium sulphate
  7. customthe solvent is removed by distillation in vacuo, together with excess malonic acid diethyl ester

出典と根拠

ORDレコード
ord-ba2bec645f404b4e94b7563d177827c9
出典データセット
uspto-grants-1984_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04430339

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