تفاعل #74719

ord-67cdaee9cec14a9bac3784b146b44a0c

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةmaintaining a temperature below 15° C
  2. 2
    درجة الحرارةto warm to room temperature
  3. 3
    استخلاصExtraction of the crude product
  4. 4
    تركيزwith chloroform and concentration

الإجراء التجريبي

2-acetyl-2,3,5-trimethoxy-2,5-dihydrofuran (9.22 g, 0.049 moles) was dissolved in 100 ml of methanol and cooled to 0° C. Solid NaBH4 (4.0 g, 0.105 moles) was added portion-wise over 1 hour, maintaining a temperature below 15° C. The reaction was then allowed to warm to room temperature, and 20 ml of saturated aqueous NH4Cl added. Extraction of the crude product with chloroform and concentration yielded 9.3 g of 2-(1-hydroxyethyl)-2,3,5-trimethoxy-2,5-dihydrofuran (100%) as a clear 0.1, NMR (CDCl3 +D2O, δ) 5.5 (1H, m), 5.03 (1H, M), 3.8 (4H, m), 3.58 (3H, s), 3.3 (3H, s), 1.10 (3H, t).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04173572uspto-grants-1979_11