Potassium Hydroxide → 9-Methylene-9H-fluorene

HRID 2253256

反応式

HRID 2253256 の反応式
O[CH2:2][CH:3]1[C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[CH:7][CH:8]=2.[OH-].[K+]>CO>[CH2:2]=[C:3]1[C:4]2[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=2)[C:10]2[C:15]1=[CH:14][CH:13]=[CH:12][CH:11]=2

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 904669H-Fluorene-9-methanol

生成物 1

HCID 781479-Methylene-9H-fluorene

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

9-Hydroxymethylfluorene (10 g) and 1 g KOH were dissolved in 90 ml of methanol and reacted at 60° C. for 1 hour, and the methanol was evaporated. From the solid thus obtained, dibenzofulvene was extracted using hexane and water, and washed with water until the hexane phase containing dibenzofulvene was neutral. After separating off the hexane phase, the hexane was evaporated, and the solid obtained was recrystallized from a mixed solvent of hexane-diethyl ether (4/6 v/v) to obtain dibenzofulvene. The melting point of the dibenzofulvene was 50-52° C.

後処理

  1. customreacted at 60° C. for 1 hour
  2. customthe methanol was evaporated
  3. customFrom the solid thus obtained
  4. extractiondibenzofulvene was extracted
  5. washwashed with water until the hexane phase
  6. additioncontaining dibenzofulvene
  7. customAfter separating off the hexane phase
  8. customthe hexane was evaporated
  9. customthe solid obtained
  10. customwas recrystallized from a mixed solvent of hexane-diethyl ether (4/6 v/v)

出典と根拠

ORDレコード
ord-ee04c424bba046deb80f0f60b96dd9f3
出典データセット
uspto-grants-2008_01
特許番号
US07323538B2

関連ノート

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