Potassium Hydroxide → HCID 21503899、化合物

HRID 1578869ノート

反応式

HRID 1578869 の反応式
[C:1]([C:6]1[CH:18]=[CH:17][C:16]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH2:9][C:8]=2[CH:7]=1)(=O)[CH2:2][CH2:3][CH3:4].[OH-].[K+].O.NN>C(O)CO>[CH2:1]([C:6]1[CH:18]=[CH:17][C:16]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH2:9][C:8]=2[CH:7]=1)[CH2:2][CH2:3][CH3:4]

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 125571201-(9H-Fluoren-2-yl)butan-1-one

生成物 1

HCID 21503899HCID 21503899、化合物

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

実験手順

A mixture of 2-butyrylfluorene (11.3 g.), powdered potassium hydroxide (4.16 g.) and 100% hydrazine hydrate (9 ml.) in ethylene glycol (104 ml.) was refluxed for 1 hour with stirring. The mixture was then slowly distilled until the boiling-point reached 185° and then heated to reflux for 3 hours. The cooled mixture was treated with water (ca. 300 ml.) and the product was isolated with ether in the usual manner. Recrystallisation from methanol gave 2-butylfluorene, m.p. 65°-66.5°.

後処理

  1. temperaturewas refluxed for 1 hour
  2. distillationThe mixture was then slowly distilled until the boiling-point
  3. customreached 185°
  4. temperatureheated
  5. temperatureto reflux for 3 hours
  6. additionThe cooled mixture was treated with water (ca. 300 ml.)
  7. customthe product was isolated with ether in the usual manner
  8. customRecrystallisation from methanol

出典と根拠

ORDレコード
ord-346d6a581bf641e0aaa63fc03bb6d299
出典データセット
uspto-grants-1976_02
特許番号
US03939276

反応ノート

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