Acetic Acid → 2,6,6-Trimethylfulvene

HRID 271026

반응식

HRID 271026 반응식
[CH3:1][C:2]1[CH2:6][CH:5]=[CH:4][CH:3]=1.[CH3:7][C:8]([CH3:10])=O.N1CCCC1.C(O)(=O)C>CCOCC.O.CO>[CH3:1][C:2]1[CH:6]=[CH:5][C:4](=[C:8]([CH3:10])[CH3:7])[CH:3]=1

참가 물질

8

반응물 4

HCID 176Acetic AcidHCID 180AcetoneHCID 31268PyrrolidineHCID 667751-Methyl-1,3-cyclopentadiene

생성물 1

HCID 143632822,6,6-Trimethylfulvene수율 92.5%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 3283Diethyl Ether용매

실험 절차

To 130 ml of dehydrated methanol, 22.6 g (283 mmol) of methylcyclopentadiene and 8.50 ml (116 mmol) of acetone were added, then 14.5 ml (174 mmol) of pyrrolidine was dropwise added at 0° C., and the mixture was reacted at room temperature for one night. Then, 10 ml (180 mmol) of acetic acid was added at 0° C. The mixture was diluted with ether and water and then subjected to extraction. Then, the organic phase was separated, washed with water and dried over anhydrous magnesium sulfate to obtain 12.9 g of a brown liquid. The analyzed values are given below.

후처리

  1. customthe mixture was reacted at room temperature for one night
  2. extractionsubjected to extraction
  3. customThen, the organic phase was separated
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate

출처 및 근거

ORD 기록
ord-02e1cd6f9c1b4900b49a714d7d59086e
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449533B2

연결된 노트

불러오는 중…