1,4-Cyclohexanedione → HCID 57805450、化合物

HRID 1644013ノート

反応式

HRID 1644013 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:11]=O)[C:5](=[CH:8][C:9]=1[F:10])[CH:6]=O.[C:13]1(=[O:20])[CH2:18][CH2:17][C:16](=[O:19])[CH2:15][CH2:14]1.[OH-].[Na+]>C(O)C>[F:1][C:2]1[C:9]([F:10])=[CH:8][C:5]2[C:4](=[CH:11][C:18]3[C:13](=[O:20])[C:14]4[C:15]([C:16](=[O:19])[C:17]=3[CH:6]=2)=[CH:11][C:4]2[C:5](=[CH:8][C:9]([F:10])=[C:2]([F:1])[CH:3]=2)[CH:6]=4)[CH:3]=1

参加物

5

反応物 3

HCID 125111,4-CyclohexanedioneHCID 14798Sodium HydroxideHCID 226289074,5-Difluorophthalaldehyde2 回

生成物 1

HCID 57805450HCID 57805450、化合物収率 65.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 4,5-difluorophthalaldehyde (Compound 22) (0.48 g, 2.8 mmol, 2 molar equivalents) and 1,4-cyclohexanedione (0.16 g, 1.4 mmol, 1 molar equivalent) in ethanol (40 ml) was added a solution of 5% aqueous NaOH (0.6 ml) at room temperature. The reaction mixture was stirred for 30 minutes at room temperature and then warmed to 60° C. After 1 hour at 60° C., the reaction mixture was cooled to room temperature. The resulting precipitate was filtered, washed with water (15 ml), ethanol (30 ml) and diethyl ether (30 ml) to give the title compound as a yellow powder (0.35 g, 64%) used as obtained.

後処理

  1. temperaturewarmed to 60° C
  2. waitAfter 1 hour at 60° C.
  3. temperaturethe reaction mixture was cooled to room temperature
  4. filtrationThe resulting precipitate was filtered
  5. washwashed with water (15 ml), ethanol (30 ml) and diethyl ether (30 ml)

出典と根拠

ORDレコード
ord-a4cac5d51f224868b5870a8bf20f1bfc
出典データセット
uspto-grants-2012_02
特許番号
US08119804B2

反応ノート

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