p-Toluenesulfonic acid → Ethyl 5,5,5-trifluoro-4-oxopentanoate

HRID 973746ノート

反応式

HRID 973746 の反応式
[F:1][C:2]([F:18])([F:17])[C:3](=[O:16])[CH:4](C(OCC)=O)[CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7].B(O)(O)O.C1(C)C=CC(S(O)(=O)=O)=CC=1>>[F:1][C:2]([F:17])([F:18])[C:3](=[O:16])[CH2:4][CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7]

参加物

4

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 7628Boric AcidHCID 11346247Butanedioic acid, (trifluoroacetyl)-, diethyl ester

生成物 1

HCID 13379932Ethyl 5,5,5-trifluoro-4-oxopentanoate収率 32.7%

実験手順

45 g of the product of Step A, 10.3 g of boric acid and 1 g of p-toluenesulfonic acid were heated at 180° C. for 3 hours and the mixture was poured into ice and extracted with ethyl acetate. The mixture was decanted, dried and concentrated under reduced pressure and the residue was distilled to obtain 10.8 g of expected product.

後処理

  1. additionthe mixture was poured into ice
  2. extractionextracted with ethyl acetate
  3. customThe mixture was decanted
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. distillationthe residue was distilled

出典と根拠

ORDレコード
ord-83ba7ad84df644098a26a657708b16de
出典データセット
uspto-grants-1991_11
特許番号
US05064861

反応ノート

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