반응 #935907

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methyl-2-methoxycarbonyl-6,6-dimethyl-6-sila-n-hexadecanoate

Methyl-2-methoxycarbonyl-6,6-dimethyl-6-sila-n-hexadecanoate

potassium hydroxide

→

title product

6,6-dimethyl-6-sila-n-hexadecanoic acid

용매

methanol

methanol

반응 조건

후처리

1. 1
   온도is refluxed for 45 min
2. 2
   농축The resulting mixture is then concentrated to a solid
3. 3
   workup.ADDITIONDilute hydrochloric acid (2N) is then added to the solid (in excess, to acid pH)
4. 4
   추출the mixture extracted with methylene chloride
5. 5
   기타The extract is dried
6. 6
   농축concentrated to a residue
7. 7
   온도The residue is heated to 160°-170° under reduced pressure (approx. 15 mm Hg), for 1 hour
8. 8
   workup.DISTILLATIONdistilled under high vacuum through a jacketed Vigreux column

실험 절차

A mixture of 6.7 g (18 mmole) of methyl-2-methoxycarbonyl-6,6-dimethyl-6-sila-n-hexadecanoate (from step C) in 50 ml of methanol and 3.0 g (about 48 mmole) of potassium hydroxide (powder) in 50 ml of methanol is refluxed for 45 min. The resulting mixture is then concentrated to a solid. Dilute hydrochloric acid (2N) is then added to the solid (in excess, to acid pH) and the mixture extracted with methylene chloride. The extract is dried, then concentrated to a residue. The residue is heated to 160°-170° under reduced pressure (approx. 15 mm Hg), for 1 hour, then distilled under high vacuum through a jacketed Vigreux column to obtain refined title product of this step (as the main fraction) at 145°-140° at 0.101-0.090 mm Hg.

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