Hydrochloric Acid → 1-(4-Fluorophenyl)-1, 4-dihydro-indeno [1, 2-c] pyrazole

HRID 366383ノート

反応式

HRID 366383 の反応式
O[CH:2]=[C:3]1[CH2:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]1=O.Cl.[F:14][C:15]1[CH:20]=[CH:19][C:18]([NH:21][NH2:22])=[CH:17][CH:16]=1.Cl>C(O)C>[F:14][C:15]1[CH:20]=[CH:19][C:18]([N:21]2[C:4]3[C:5]4[C:10]([CH2:11][C:3]=3[CH:2]=[N:22]2)=[CH:9][CH:8]=[CH:7][CH:6]=4)=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 699814-Fluorophenylhydrazine hydrochlorideHCID 37648821H-Inden-1-one, 2,3-dihydro-2-(hydroxymethylene)-

生成物 1

HCID 122910661-(4-Fluorophenyl)-1, 4-dihydro-indeno [1, 2-c] pyrazole

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-Hydroxymethylene indan-1-one, (Example 1(ii) (a) (4.004 g; 250 mmol), p-fluorophenyl hydrazine hydrochloride (Aldrich) (4.106 g; 25.25 mmol) 10M hydrochloric acid (1 cm3) and ethanol (30 cm3), were heated under reflux for 19 hours. After cooling, the solvent was evaporated under reduced pressure, then taken up in dichloromethane and washed with 2M NaOH. The organic layer was separated, dried (Na2SO4), filtered and concentrated in vacuo. Purification by Kugelrohr distillation (140° C.; 0.01 mmHg) afforded a yellow solid, m.p. 104-105° C.

後処理

  1. temperatureunder reflux for 19 hours
  2. temperatureAfter cooling
  3. customthe solvent was evaporated under reduced pressure
  4. washwashed with 2M NaOH
  5. customThe organic layer was separated
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customPurification
  10. distillationby Kugelrohr distillation (140° C.; 0.01 mmHg)
  11. customafforded a yellow solid, m.p. 104-105° C.

出典と根拠

ORDレコード
ord-538bde8ff3034153b72fd8cf2836b91c
出典データセット
uspto-grants-2000_10
特許番号
US06130228

反応ノート

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