反应详情

Methanesulphonyl chloride (74.0 g) was added dropwise over 30 minutes to a solution of 2-hydroxymethyl-2-n-propylpropan-1,3-diol 2× 2× 2-hydroxymethyl-2-n-propyl g) (m.pt. (28.0 g) in dry pyridine (200 ml) under nitrogen at 0° C. The mixture was allowed to warm to room temperature. After stirring for 18 hours the mixture was poured into water (200 ml) and extracted with chloroform (2 × 200 ml). The chloroform extracts were washed with water (2 × 100 ml), dried over anhydrous magnesium sulphate and evaporated in vacuo to give a brown solid. This was stirred in dry diethyl ether (200 ml) to give 2-hydroxymethyl-2-n-propyl propan-1,3-diol trimethanesulphonate as a white solid. (70.0 g)(m.pt.103.6°).

1. customat 0° C
2. extractionextracted with chloroform (2 × 200 ml)
3. washThe chloroform extracts were washed with water (2 × 100 ml)
4. dry with materialdried over anhydrous magnesium sulphate
5. customevaporated in vacuo
6. customto give a brown solid