Acetic Acid → 1-(2,6,6-Trimethylcyclohex-3-en-1-yl)but-2-en-1-one

HRID 8564

반응식

HRID 8564 반응식
[CH3:1][CH:2]1[CH:7]=[CH:6][CH2:5][C:4]([CH3:9])([CH3:8])[CH:3]1[CH2:10][CH:11]=O.[CH:13](=O)[CH3:14].C(O)(=[O:18])C.O>C(OCCCC)(=O)C>[CH3:1][CH:2]1[CH:7]=[CH:6][CH2:5][C:4]([CH3:9])([CH3:8])[CH:3]1[C:10](=[O:18])[CH:11]=[CH:13][CH3:14]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 177AcetaldehydeHCID 962WaterHCID 219833661-(2,6,6-Trimethyl-3-cyclohexen-1-yl)-2-ethanone

생성물 1

HCID 422961-(2,6,6-Trimethylcyclohex-3-en-1-yl)but-2-en-1-one

시약·촉매·용매 1

HCID 31272Butyl Acetate용매2회

반응 조건

온도
100 °C

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.

후처리

  1. customas prepared above and a quantity
  2. additionwere introduced under the surface of the liquid, over 3 hours
  3. temperatureAfter the completion of the introduction the reaction was cooled to 35° C
  4. customTo the cooled reaction medium
  5. stirringAfter stirring a few minutes
  6. customthe water phase was removed
  7. washby washing it with 25 g of 20% aqueous potassium carbonate

출처 및 근거

ORD 기록
ord-abb76655ac01447ea0ff9d306d69fe0b
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091151B2

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