Hydrochloric Acid → HCID 66839325、化合物

HRID 546790ノート

反応式

HRID 546790 の反応式
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][C:10]([O:12][CH3:13])=[O:11].CC(C)([O-])C.[K+].Br[CH2:23][CH2:24][C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26].Cl>C1COCC1>[CH3:13][O:12][C:10](=[O:11])[CH:9]([C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[C:2]([F:14])([F:15])[F:1])[CH2:23][CH2:24][C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 256128tert-Butyl 3-bromopropionateHCID 23294844Methyl [2-(trifluoromethyl)phenyl]acetateHCID 23665647Potassium tert-butoxide

生成物 1

HCID 66839325HCID 66839325、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Methyl 2-trifluoromethylphenylacetate (5 g) was dissolved in THF (75 mL). Potassium tert-butoxide (2.71 g) was added under ice-cooling, and the reaction solution was stirred for 30 minutes. tert-Butyl 3-bromopropionate (3.83 mL) was added to the reaction solution. The reaction solution was gradually heated until room temperature and stirred for four hours. A 1 N hydrochloric acid aqueous solution was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (carrier: Chromatorex Si; elution solvent: heptane:ethyl acetate=19:1→heptane:ethyl acetate=1:1) to obtain the title compound (6 g). The property values of the compound are as follows.

後処理

  1. temperaturecooling
  2. stirringstirred for four hours
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by silica gel chromatography (carrier: Chromatorex Si; elution solvent: heptane:ethyl acetate=19:1→heptane:ethyl acetate=1:1)

出典と根拠

ORDレコード
ord-67194a7a11e64cd1af377858e7f89211
出典データセット
uspto-grants-2011_05
特許番号
US07935815B2

反応ノート

読み込み中…