반응 #1162810

반응 방정식

methyl [5-(3,5,5,8,8-pentamethyl-2,3,5,6,7,8-hexahydronaphtho[2,3-b]furan-3-yl)-thiophene-3-yl]carboxylate

lithium hydroxide

methanol

water

→

[5-(3,5,5,8,8-pentamethyl-2,3,5,6,7,8-hexahydronaphtho[2,3-b]furan-3-yl)thiophene-3-yl]carboxylic acid

용매

THF

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux for 6 h
3. 3
   농축After concentrating in a rotary evaporator under vacuum at 40° C.
4. 4
   workup.ADDITIONadding water, ethyl ether and acidifying with a concentrated hydrochloric acid solution to pH 1
5. 5
   세척the organic phase was washed twice with water
6. 6
   건조dried over magnesium sulfate
7. 7
   농축concentrated in a rotary evaporator under vacuum at 40° C
8. 8
   기타The solids obtained
9. 9
   세척were washed with heptane

실험 절차

A mixture of methyl [5-(3,5,5,8,8-pentamethyl-2,3,5,6,7,8-hexahydronaphtho[2,3-b]furan-3-yl)-thiophene-3-yl]carboxylate (2.1 g, 5.4 mmol), lithium hydroxide (2g, 48 mmol), methanol (1 ml) and water (1 ml) in 30 ml of THF was heated under reflux for 6 h. After concentrating in a rotary evaporator under vacuum at 40° C., adding water, ethyl ether and acidifying with a concentrated hydrochloric acid solution to pH 1, the organic phase was washed twice with water, dried over magnesium sulfate and concentrated in a rotary evaporator under vacuum at 40° C. The solids obtained were washed with heptane.

출처