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

HRID 916044노트

반응식

HRID 916044 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5a60ab55f63f4f6797f9db83a417b27a
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07268152B2

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