Formic Acid → 4-(4-Ethoxy-2,3-difluorophenyl)cyclohexanone

HRID 2120500노트

반응식

HRID 2120500 반응식
C1O[C:4]2([CH2:9][CH2:8][CH:7]([C:10]3[CH:15]=[CH:14][C:13]([O:16][CH2:17][CH3:18])=[C:12]([F:19])[C:11]=3[F:20])[CH2:6][CH2:5]2)[O:3]C1.C(O)=O>C1(C)C=CC=CC=1>[F:20][C:11]1[C:12]([F:19])=[C:13]([O:16][CH2:17][CH3:18])[CH:14]=[CH:15][C:10]=1[CH:7]1[CH2:8][CH2:9][C:4](=[O:3])[CH2:5][CH2:6]1

참가 물질

4

반응물 2

HCID 284Formic AcidHCID 220205208-(2,3-Difluoro-4-ethoxyphenyl)-1,4-dioxaspiro[4.5]decane

생성물 1

HCID 111611214-(4-Ethoxy-2,3-difluorophenyl)cyclohexanone수율 100%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Crude 4-(2,3-difluoro-4-ethoxyphenyl)-cyclohexanone monoethylene acetal (50.3 mmol) obtained in Step 1 was dissolved in 200 ml of toluene, 87% formic acid (503 mmol) was added, and the solution was heated to reflux for 4 hours. The reaction solution was washed twice with 100 ml of a saturated aqueous solution of sodium hydrogen carbonate, then three times with 100 ml of water, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, to form crude 4-(2,3-difluoro-4-ethoxyphenyl)-cyclohexanone (50.3 mmol).

후처리

  1. temperaturethe solution was heated
  2. temperatureto reflux for 4 hours
  3. washThe reaction solution was washed twice with 100 ml of a saturated aqueous solution of sodium hydrogen carbonate
  4. dry with materialthree times with 100 ml of water, and dried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-493bf51639fe4947b892441bb96492d4
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06692657B1

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