Formic Acid → HCID 178466567、化合物

HRID 1793274ノート

反応式

HRID 1793274 の反応式
[F:1][C:2]1[C:7]([F:8])=[C:6]([O:9][CH2:10][CH3:11])[CH:5]=[CH:4][C:3]=1[C@H:12]1[CH2:17][CH2:16][C@H:15]([CH2:18][CH2:19][CH:20]2OCCC[O:21]2)[CH2:14][CH2:13]1.C(O)=O>C1(C)C=CC=CC=1>[F:1][C:2]1[C:7]([F:8])=[C:6]([O:9][CH2:10][CH3:11])[CH:5]=[CH:4][C:3]=1[C@H:12]1[CH2:17][CH2:16][C@H:15]([CH2:18][CH2:19][CH:20]=[O:21])[CH2:14][CH2:13]1

参加物

4

反応物 2

HCID 284Formic AcidHCID 178466566HCID 178466566、化合物

生成物 1

HCID 178466567HCID 178466567、化合物収率 100%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

The 2-(2-(trans-4-(2,3-difluoro-4-ethoxyphenyl)-cyclohexyl)-ethyl)-1,3-dioxane (19.8 mmol) obtained by the reaction of Step 4 was dissolved in 100 ml of toluene, 87% formic acid (198 mmol) was added, and the solution was heated to reflux for 4 hours. The reaction solution was twice washed with 50 ml of a saturated aqueous solution of sodium hydrogen carbonate, then three times with 50 ml of water, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, to form crude 3-(trans-4-(2,3-difluoro-4-ethoxyphenyl)-cyclohexyl)-propanal (19.8 mmol).

後処理

  1. temperaturethe solution was heated
  2. temperatureto reflux for 4 hours
  3. washThe reaction solution was twice washed with 50 ml of a saturated aqueous solution of sodium hydrogen carbonate
  4. dry with materialthree times with 50 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-c5d2a3c98a094bf9b2875bcfff8c573c
出典データセット
uspto-grants-2006_07
特許番号
US07081279B2

反応ノート

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