반응 #8660

ord-abb76655ac01447ea0ff9d306d69fe0b

반응 방정식

O
water
CC1C=CCC(C)(C)C1CC=O
1-(2,6,6-trimethyl-3-cyclohexen-1-yl)-2-ethanone
CC=O
acetaldehyde
CC(=O)O
acetic acid
CC=CC(=O)C1C(C)C=CCC1(C)C
1-(2,6,6-trimethyl-3-cyclohexen-1-yl)-2-buten-1-one

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타as prepared above and a quantity
  2. 2
    workup.ADDITIONwere introduced under the surface of the liquid, over 3 hours
  3. 3
    온도After the completion of the introduction the reaction was cooled to 35° C
  4. 4
    기타To the cooled reaction medium
  5. 5
    workup.STIRRINGAfter stirring a few minutes
  6. 6
    기타the water phase was removed
  7. 7
    세척by washing it with 25 g of 20% aqueous potassium carbonate

실험 절차

In a 250 ml flask were added 30 g (0.18 mole) of 1-(2,6,6-trimethyl-3-cyclohexen-1-yl)-2-ethanone (94% purity), 12.0 g of butyl acetate, an aliquot according to Table 1 of the catalytic solution as prepared above and a quantity of co-ingredient according to Table 1. The resulting mixture was stirred at 100° C. To said mixture, 4.0 g (0.09 mole) of acetaldehyde, diluted in 10 g of butyl acetate were introduced under the surface of the liquid, over 3 hours. After the completion of the introduction the reaction was cooled to 35° C. To the cooled reaction medium were added 10 g of acetic acid and then 40 ml of water. After stirring a few minutes, the water phase was removed and the organic phase was neutralized by washing it with 25 g of 20% aqueous potassium carbonate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091151B2uspto-grants-2006_08