Acetone → 2,6,6-Trimethylfulvene

HRID 2216718ノート

反応式

HRID 2216718 の反応式
[CH3:1][C:2]1[CH:6]=[CH:5][CH2:4][CH:3]=1.[CH3:7][C:8]([CH3:10])=O.N1CCCC1.OP(O)(O)=O>C(O)C>[CH3:1][C:2]1[CH:3]=[CH:4][C:5](=[C:8]([CH3:10])[CH3:7])[CH:6]=1

参加物

6

反応物 4

HCID 180AcetoneHCID 1004Phosphoric AcidHCID 31268PyrrolidineHCID 1380262-Methylcyclopentadiene

生成物 1

HCID 143632822,6,6-Trimethylfulvene

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-methyl-1,3-cyclopentadiene (125 g, 1.56 mol) in 1.2 L of ethanol was treated at low temperature with 126 mL (1.72 mol) of acetone and 142 mL (1.72 mol) of pyrrolidine. The resulting solution was kept below room temperature overnight. Then the reaction mixture was neutralized with a 10% aq. solution of H3PO4, extracted with hexane (3×150 mL) and washed with water until neutral pH. The organic phase was separated, dried with MgSO4 and concentrated. The residue was distilled at 70° C./60 mmHg. Yield 112.6 g (60%).

後処理

  1. extractionextracted with hexane (3×150 mL)
  2. washwashed with water until neutral pH
  3. customThe organic phase was separated
  4. dry with materialdried with MgSO4
  5. concentrationconcentrated
  6. distillationThe residue was distilled at 70° C./60 mmHg

出典と根拠

ORDレコード
ord-0ea6ee23bbb54644b791afdbeddc273d
出典データセット
uspto-grants-2006_09
特許番号
US07112638B2

反応ノート

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