تفاعل #74986

معادلة التفاعل

1[7-[(1,3-dithia-2-cyclopentyl)]-3,3-dimethyl-1,5-dioxaspiro[5,4]-dec-8-yl]-trans-1-octene-3-ol tetrahydropyranyl ether

methyl iodide

CaCO3

H2O

DMF

→

3-[3,3-Dimethyl-8[-3-pentyl-3-tetrahydropyranyloxy-trans-1-propenyl]-1,5-dioxaspiro[5,4]-dec-7-yl]-propionaldehyde

المذيبات

acetone

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe solution was cooled
2. 2
   ترشيحfiltered with suction
3. 3
   أخرىto remove the precipitate
4. 4
   أخرىthe filtrate was evaporated to dryness at 0.1 mm Hg
5. 5
   workup.DISSOLUTIONThe residue was dissolved in ether
6. 6
   غسيلwashed with H2O
7. 7
   تجفيفdried over MgSO4
8. 8
   أخرىthe solvent was removed by distillation under reduced pressure
9. 9
   أخرىThe oily residue which was not further purified

الإجراء التجريبي

1.05 g [2.05 mmoles] of 1[7-[(1,3-dithia-2-cyclopentyl)]-3,3-dimethyl-1,5-dioxaspiro[5,4]-dec-8-yl]-trans-1-octene-3-ol-tetrahydropyranyl ether was stirred for 2 hours at 50° C. in 100 ml of DMF with 0.7 ml (10.3 mmoles) of methyl iodide, 1.4 g (14 moles) of CaCO3 and 0.4 ml of H2O. The solution was cooled, combined with 50 ml of acetone, filtered with suction to remove the precipitate and the filtrate was evaporated to dryness at 0.1 mm Hg. The residue was dissolved in ether, washed with H2O, dried over MgSO4 and the solvent was removed by distillation under reduced pressure. The oily residue which was not further purified showed in the infrared spectrum a strong carbonyl band at 1730 cm-1.

المصدر