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

HRID 2120500ノート

反応式

HRID 2120500 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-493bf51639fe4947b892441bb96492d4
出典データセット
uspto-grants-2004_02
特許番号
US06692657B1

反応ノート

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