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Hydrochloric Acid → (-)-Ethyl mandelate

HRID 2166209
ノート
印刷プレビュー

反応式

HRID 2166209 の反応式
C(O)(=O)[C@@H]([C@H](C(O)=O)O)O.[C:11]1([C:17](=[O:23])[C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[Na].Cl>C1COCC1>[OH:23][C@H:17]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:18]([O:20][CH2:21][CH3:22])=[O:19]
参加物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 313Hydrochloric AcidHCID 15349Ethyl benzoylformateHCID 444305L-Tartaric acidHCID 5360545Sodium

生成物 1

HCID 6951556(-)-Ethyl mandelate収率 85.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 1.70 g (11.3 mmol) of L-(+)-tartaric acid in 35 ml of THF was cooled in a cryostat at -20° C., and a solution of 0.5 g (2.8 mmol) of ethyl phenylglyoxylate in THF (5 ml) was added. To the resulting solution, there was further added 0.43 g (11.3 mmol) of sodium borohyride, all at once and with stirring, and the mixture was stirred for 24 hours. The reaction mixture was cooled in an ice bath, 20 ml of 1N HCl was added, and stirring was continued for 15 minutes. After distilling off THF under reduced pressure, the aqueous layer was extracted twice with ethyl acetate (30 ml and 20 ml), and the combined extract was washed first with 20 ml of a saturated aqueous solution of sodium chloride, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure from the dried solution, and the residue was purified by silica gel column chromatography, giving 0.43 g of ethyl (R)-(-)-2-hydroxy-2-phenylacetate as an ethyl acetate:n-hexane fraction(1:5). Its specific rotation [α]D16 was -108.4° (cl. 12, CHCl3). The synthesis yield was 85% and the optical yield was 85% e.e (see Reference 7).

後処理

  1. stirringthe mixture was stirred for 24 hours
  2. temperatureThe reaction mixture was cooled in an ice bath
  3. stirringstirring
  4. distillationAfter distilling off THF under reduced pressure
  5. extractionthe aqueous layer was extracted twice with ethyl acetate (30 ml and 20 ml)
  6. extractionthe combined extract
  7. washwas washed first with 20 ml of a saturated aqueous solution of sodium chloride
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationThe solvent was distilled off under reduced pressure from the dried solution
  10. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-0bafa9df0942487d9afe224a0e3c8b69
出典データセット
uspto-grants-1990_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04943652

反応ノート

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