1,4-Cyclohexanedione → HCID 57805450, 화합물

HRID 2104939노트

반응식

HRID 2104939 반응식
[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

참가 물질

5

반응물 3

HCID 125111,4-CyclohexanedioneHCID 14798Sodium HydroxideHCID 226289074,5-Difluorophthalaldehyde2회

생성물 1

HCID 57805450HCID 57805450, 화합물수율 65.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-309e2277b6294e41b8a563b0496216d1
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576208B2

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