Vinyl isobutyl ether → HCID 70388635、化合物

HRID 248860

反応式

HRID 248860 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 70388635HCID 70388635、化合物収率 30.7%

試薬・触媒・溶媒 1

HCID 785Hydroquinone触媒

反応条件

温度
220 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-271966fa3bd34eb7b7b40b0f1c058e96
出典データセット
uspto-grants-1993_05
特許番号
US05212183

関連ノート

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