1,4-Cyclohexanedione → HCID 57805450、化合物

HRID 2104939ノート

反応式

HRID 2104939 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-309e2277b6294e41b8a563b0496216d1
出典データセット
uspto-grants-2009_08
特許番号
US07576208B2

反応ノート

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