Fluorene-1-carboxylic acid → 1-Fluorenemethanol

HRID 1089847

反応式

HRID 1089847 の反応式
[C:1]1([C:14](O)=[O:15])[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1>C1COCC1>[C:1]1([CH2:14][OH:15])[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1

参加物

3

反応物 1

HCID 80468Fluorene-1-carboxylic acid

生成物 1

HCID 523071-Fluorenemethanol収率 68.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 1-fluorenecarboxylic acid (10.0 g, 47.6 mmol) in THF (150 mL) at 0° C. was charged With a 1M solution of BH3 -THF complex in THF (80 mL, 80 mmol). The reaction mixture was stored overnight at room temperature then quenched with 30 mL of 10% AcOH in methanol. After dilution with water (100 mL), the water layer was extracted with ethyl acetate (3×50 mL). The combined organic extracts were washed with 10% potassium carbonate solution, water, brine, dried over magnesium sulfate and evaporated. The residue (white crystals) was washed with ether and dried to afford 1-fluorenemethanol (6.4 g, 68.5%).

後処理

  1. customthen quenched with 30 mL of 10% AcOH in methanol
  2. extractionAfter dilution with water (100 mL), the water layer was extracted with ethyl acetate (3×50 mL)
  3. washThe combined organic extracts were washed with 10% potassium carbonate solution, water, brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. washThe residue (white crystals) was washed with ether
  7. customdried

出典と根拠

ORDレコード
ord-d4abbb86065b4b868f48615ea64e945e
出典データセット
uspto-grants-1992_01
特許番号
US05079260

関連ノート

読み込み中…