Hydrochloric Acid → 3-(2,3-Dihydro-1-benzofuran-7-yl)-3-methylbutanoic acid

HRID 916044ノート

反応式

HRID 916044 の反応式
[O:1]1[C:5]2[C:6]([C:10]([CH3:19])([CH3:18])[CH2:11][C:12](=[O:17])C(F)(F)F)=[CH:7][CH:8]=[CH:9][C:4]=2[CH2:3][CH2:2]1.[OH-:20].[Na+].Cl>C(OCC)(=O)C>[O:1]1[C:5]2[C:6]([C:10]([CH3:19])([CH3:18])[CH2:11][C:12]([OH:17])=[O:20])=[CH:7][CH:8]=[CH:9][C:4]=2[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 469392134-(2,3-Dihydrobenzofur-7-yl)-1,1,1-trifluoro-4-methyl-2-pentanone

生成物 1

HCID 589600353-(2,3-Dihydro-1-benzofuran-7-yl)-3-methylbutanoic acid収率 99%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

4-(2,3-Dihydrobenzofur-7-yl)-1,1,1-trifluoro-4-methyl-2-pentanone (1.00 g) was treated with NaOH (3.6 mL, 4 M in ethanol-water (2:1)) at room temperature. The mixture was heated to 80° C. for 1 hour. After the mixture had been cooled to room temperature, 20 mL of ethyl acetate, and approximately 15 mL of 2 M HCl were added. The organic phase was separated and the aqueous layer was extracted with three 20 mL portions of ethyl acetate. The combined organic phases were dried over magnesium sulfate. The solvent was removed to yield 800 mg (99%) of 3-(2,3-dihydrobenzofur-7-yl)-3-methylbutanoic acid as an orange-brown solid.

後処理

  1. temperatureAfter the mixture had been cooled to room temperature
  2. customThe organic phase was separated
  3. extractionthe aqueous layer was extracted with three 20 mL portions of ethyl acetate
  4. dry with materialThe combined organic phases were dried over magnesium sulfate
  5. customThe solvent was removed

出典と根拠

ORDレコード
ord-5a60ab55f63f4f6797f9db83a417b27a
出典データセット
uspto-grants-2007_09
特許番号
US07268152B2

反応ノート

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