Butanedione → HCID 22320020, 화합물

HRID 497578노트

반응식

HRID 497578 반응식
[CH:1]12[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][CH:4]([CH2:5]3)[O:3][C:2]1=[O:12])[CH2:9]2.C[C:14](=O)[C:15](=[O:17])C.O=O>C(O)(=O)C>[C:15]([C:6]12[CH2:11][CH:1]3[CH2:9][CH:8]([CH2:10][CH:4]([O:3][C:2]3=[O:12])[CH2:5]1)[CH2:7]2)(=[O:17])[CH3:14]

참가 물질

5

반응물 3

HCID 650ButanedioneHCID 977OxygenHCID 5567274-Oxatricyclo[4.3.1.13,8]undecan-5-one

생성물 1

HCID 22320020HCID 22320020, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
80 °C

실험 절차

In a flask were placed 3-oxatricyclo[4.3.1.14,8]undecan-2-one (16.6 g, 100 mmol), acetylacetonatocobalt [Co(acac)2] (50 mmol), 2,3-butanedione (600 mmol), and acetic acid (100 g). A condenser and an oxygen balloon were attached to the flask, and the mixture in the flask was vigorously stirred at 80° C. for 4 hours. After the completion of the reaction, the reaction mixture was concentrated, followed by addition of toluene and washing with water. The resulting organic layer was concentrated, the concentrate was subjected to silica gel column chromatography and thereby yielded the title compound 6-acetyl-3-oxatricyclo[4.3.1.14,8]undecan-2-one in a yield of 37%.

후처리

  1. customIn a flask were placed
  2. customAfter the completion of the reaction
  3. concentrationthe reaction mixture was concentrated
  4. additionfollowed by addition of toluene
  5. washwashing with water
  6. concentrationThe resulting organic layer was concentrated

출처 및 근거

ORD 기록
ord-213326070c114b72a4f86b8e608c703b
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949615B2

반응 노트

불러오는 중…