Triethylamine → HCID 11275184, 화합물

온도

30 °C

1035 g (11 mol) of acetaldehyde dimethyl acetal [purity according to gas chromatography (GC): 96.5%] and 3.4 g (3 ml, 24 mmol, 0.22 mol %) of boron trifluoride etherate were placed under argon in a 2 l two-necked round flask fitted with a magnetic stirrer, a thermometer and a dropping funnel. 530 g (7.35 mol) of methyl (1-propenyl) ether were added dropwise to the mixture within 2 hours at between 30° and 40° C. with occasional cooling (the reaction was exothermic). After completion of the addition the mixture was stirred for a further 30 minutes at 30° C., then cooled to room temperature. 3 ml of triethylamine were added thereto, the mixture was stirred for 15 minutes and suction filtered. The excess acetaldehyde dimethyl acetal was then distilled off on a Raschig column (50×3 cm) at normal pressure and the residue was fractionated on the same column. This gave at a pressure of 50 mbar a 1st fraction (b.p. 81.5°-83.5° C.) consisting of 742 g (60% yield) of 1,1,3-trimethoxy-2-methyl-butane (content according to GC: 96.4%) as a colourless liquid and a 2nd fraction (b.p. 83.5°-85° C.) consisting of 87.5 g (6.3% yield) of 1,1,3-trimethoxy-2-butane (content according to GC: 86%), likewise as a colourless liquid, i.e. a total yield of 66.3% of the desired product.

1. customfitted with a magnetic stirrer
2. temperaturewith occasional cooling (the reaction
3. additionAfter completion of the addition the mixture
4. temperaturecooled to room temperature
5. stirringthe mixture was stirred for 15 minutes
6. filtrationsuction filtered
7. distillationThe excess acetaldehyde dimethyl acetal was then distilled off on a Raschig column (50×3 cm) at normal pressure
8. customThis gave at a pressure of 50 mbar a 1st fraction (b.p. 81.5°-83.5° C.)

ORD 기록

ord-942c2b4bc9a34127ad07bac468c1d46a

출처 데이터셋

uspto-grants-1998_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US05786518