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Ethyl 2-[4-(2,4-dichlorophenoxy)phenoxy]propanoate → HCID 12804883、化合物

HRID 224220
ノート
印刷プレビュー

反応式

HRID 224220 の反応式
C([O:3][C:4](=O)[CH:5]([O:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:16]=2[Cl:22])=[CH:10][CH:9]=1)[CH3:6])C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C(OCC)C>[Cl:22][C:16]1[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=1[O:14][C:11]1[CH:12]=[CH:13][C:8]([O:7][CH:5]([CH3:6])[CH2:4][OH:3])=[CH:9][CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 12952858Ethyl 2-[4-(2,4-dichlorophenoxy)phenoxy]propanoateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 12804883HCID 12804883、化合物収率 94.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

48 g of ethyl-α-[4-(2,4-dichlorophenoxy)phenoxy]propionate was dissolved in 80 ml of anhydrous diethyl ether and the solution was added dropwise to a dispersion of 5 g of lithium aluminum hydride in 200 ml of anhydrous diethyl ether while cooling. After completion of the addition, the mixture was allowed to stand for 12 hours at room temperature and then heated under refluxing for 1.5 hours to complete the reaction. The reaction mixture was poured into an appropriate amount of ice water, and the ethereal layer was separated. The ethereal layer was again extracted with diethyl ether and the extract was dried over anhydrous sodium sulfate. The ether was removed by distillation from the dried extract, and the residue was distilled under reduced pressure to obtain 40 g of the desired product having a boiling point of 201° to 205° C./2 mmHg.

後処理

  1. temperaturewhile cooling
  2. additionAfter completion of the addition
  3. temperatureheated
  4. temperatureunder refluxing for 1.5 hours
  5. customthe reaction
  6. customthe ethereal layer was separated
  7. extractionThe ethereal layer was again extracted with diethyl ether
  8. dry with materialthe extract was dried over anhydrous sodium sulfate
  9. customThe ether was removed by distillation from the dried
  10. extractionextract
  11. distillationthe residue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-18b989c0606549ca8611f6776460b122
出典データセット
uspto-grants-1980_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04231787

反応ノート

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