تفاعل #73466

معادلة التفاعل

[1-Methyl-1-(4-oxo-cyclohexyl)-ethyl]-carbamic acid tert-butyl ester

sodium borohydride

→

( 21 )

المردود 93.4%

[1-Methyl-1-(4-hydroxy-cyclohexyl)-ethyl]carbamic acid tert-butyl ester

المردود 93.4%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   أخرىThe mixture was evaporated
2. 2
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
3. 3
   غسيلwashed twice with 2N hydrochloric acid and once with brine
4. 4
   تجفيفThe organic layer was dried over sodium sulphate
5. 5
   أخرىevaporated to dryness

الإجراء التجريبي

2.91 g of [1-Methyl-1-(4-oxo-cyclohexyl)-ethyl]-carbamic acid tert-butyl ester (20) were dissolved in 60 mL of ethanol and 473 mg of sodium borohydride were added at −20° C. The mixture was allowed to warm to room temperature and stirred for 3.5 h. The mixture was evaporated, the residue was dissolved in ethyl acetate and washed twice with 2N hydrochloric acid and once with brine. The organic layer was dried over sodium sulphate and evaporated to dryness to give 2.74 g of (21). Rt=1.27 min (Method 5). Detected mass: 194 (M-Isobutene-H2O+H+).

المصدر