Acetic Acid → 2-Methylene-octanal

HRID 2243791

반응식

HRID 2243791 반응식
[C:1](O)(=O)C.O.[CH:6](=[O:14])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]>C=O>[CH2:1]=[C:7]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[CH:6]=[O:14]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 454OctanalHCID 962Water

생성물 1

HCID 112057952-Methylene-octanal

시약·촉매·용매 1

HCID 712Formaldehyde용매

반응 조건

온도
50 °C

실험 절차

A 5-liter flask fitted with an overhead stirrer and condenser was charged with di-N-butyl amine (61 g, 0.47 mol) and acetic acid (56 g, 0.9 mol). Roughly 900 ml of 37% formaldehyde solution in water (351 g formaldehyde, 11.7 mol) was then added and the resulting solution was heated to 50° C. with stirring. After this temperature was reached octanal (1000 g, 7.0 mol) was fed in over about 2 h. A slight exotherm was noticed during the feed. Monitoring by GC showed the consumption of octanal and the production of 2-methylene octanal, finally reaching roughly 95% conversion after the addition was complete. The reaction mixture was allowed to cool to room temperature, poured into a separatory funnel, and washed once with 5% HCl solution. The organic layer was then washed once with saturated sodium bicarbonate, then taken directly on to the next step.

후처리

  1. customA 5-liter flask fitted with an overhead stirrer and condenser
  2. customwas fed in over about 2 h
  3. customthe consumption of octanal
  4. additionafter the addition
  5. temperatureto cool to room temperature
  6. additionpoured into a separatory funnel
  7. washwashed once with 5% HCl solution
  8. washThe organic layer was then washed once with saturated sodium bicarbonate

출처 및 근거

ORD 기록
ord-5716b618c32145f9a2b7e53108cf8036
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07678749B2

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