Vinyl isobutyl ether → HCID 70388635, 화합물

HRID 248860

반응식

HRID 248860 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([CH:11]=[C:12]([CH3:15])[CH:13]=[O:14])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[CH2:16]([O:20][CH:21]=[CH2:22])[CH:17]([CH3:19])[CH3:18]>C1(C=CC(O)=CC=1)O>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([C:11]2[CH2:22][CH:21]([O:20][CH2:16][CH:17]([CH3:19])[CH3:18])[O:14][CH2:13][C:12]=2[CH3:15])=[CH:9][CH:10]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

반응물 2

HCID 7992Vinyl isobutyl etherHCID 1146592-Propenal, 3-[4-(1,1-dimethylethyl)phenyl]-2-methyl-

생성물 1

HCID 70388635HCID 70388635, 화합물수율 30.7%

시약·촉매·용매 1

HCID 785Hydroquinone촉매

반응 조건

온도
220 °C

실험 절차

3,000 g of 3-(4-tert.-butylphenyl)-2-methylprop-2-enal III and 2,000 g of vinyl isobutyl ether IV are introduced into a 10 l stirred autoclave, and 5 g of hydroquinone are added to the reaction mixture for stabilization. The autoclave is closed and then flushed with nitrogen, after which it is heated to 220° C., maintained under these conditions for 18 hours and then let down and opened. The reaction mixture (4,855 g) consists of about 39.6% of the desired product V. When the reaction mixture is worked up by fractionation in a laboratory column containing 10 sieve trays, a total of 1,379 g of the compound V of boiling point 135°-146° C. under 2 mbar are obtained from the 1,923 g shown to be present in the crude mixture by gas chromatographic analysis. This corresponds to a yield of 23%, based on the starting material III employed. 1,745 g of III, which contains some product V, are recovered. The last-mentioned amounts are reused for the reaction with vinyl isobutyl ether.

후처리

  1. additionare added to the reaction mixture for stabilization
  2. customThe autoclave is closed
  3. customflushed with nitrogen
  4. temperaturemaintained under these conditions for 18 hours
  5. additioncontaining 10 sieve trays

출처 및 근거

ORD 기록
ord-271966fa3bd34eb7b7b40b0f1c058e96
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05212183

연결된 노트

불러오는 중…