Hydrochloric Acid → Diethyl benzylsuccinate

HRID 483382ノート

反応式

HRID 483382 の反応式
[C:1]1([CH2:7][C:8](C(OCC)=O)([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl>>[C:1]1([CH2:7][CH:8]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

3

反応物 2

HCID 313Hydrochloric AcidHCID 563419Triethyl 3-phenyl-1,2,2-propanetricarboxylate

生成物 1

HCID 576172Diethyl benzylsuccinate収率 84.7%

実験手順

A solution of the product from step (a) (23.6 g) in c.HCl (326 ml) was stirred under reflux for 46 hours, then cooled. The resulting precipitate was extracted with chloroform (×3) and the extracts combined, washed with 2M aqu. KOH (×2), acidified to pH 4.0 (2M aqu. HCl) and cooled. The resulting precipitate was filtered off, washed with water and dried in vacuo to give the desired product (15.7 g). The 200 MHz 1H NMR was consistent with the proposed structure.

後処理

  1. temperatureunder reflux for 46 hours
  2. temperaturecooled
  3. extractionThe resulting precipitate was extracted with chloroform (×3)
  4. washwashed with 2M aqu
  5. temperaturecooled
  6. filtrationThe resulting precipitate was filtered off
  7. washwashed with water
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-bc07f67c065949cfb8820a459ba7ce85
出典データセット
uspto-grants-1993_07
特許番号
US05225431

反応ノート

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