g 92 tlc showed one spot r f 0 58 1 1 methanol acetone ir kbr 3500 3200 br 2950 1660 1460 1410 1340 1300 1225 1180 1140 1095 1020 960 880 860 and 800 cm 1 1 hnmr d 2 o u03b4 4 20 3 90 m 3 70 m 3 20 2 72 m 2 60 2 20 m 2 08 1 44 m anal calcd for c 7 h 15 o 4 s 3 na 0 75 h 2 o c 28 42 h 5 61 s 32 51 found c 28 68 h 5 18 s 32 05 for c 7 h 15 o 4 s 3 na 1 15 h 2 o u2192 c 7 h 15 o 4 s 3 na 0 75h 2 o calcd for h 2 o 2 37 found 2 30 a solution of 1 2 dithiopane 1 1 dioxide 1 22 g 8 84 mmol in methylene chloride 5 ml was added dropwise 1 min to a stirred solution of 3 mercaptopropionic acid 0 80 g 7 54 mmol and sodium 0 17 g 7 40 mg atom in methanol 25 ml at 5 u00b0 c after the solution was stirred for 5 min the disulfide sulfinate salt b was precipitated by the addition of acetone 300 ml solvent was decanted and the white precipitate was redissolved in a minimum amount of methanol ca 10 ml acetone ca 10 ml again was added until some precipitate ca 10 20 of sample weight resulted this mixture was centrifuged and the clear solution so obtained was removed and diluted with sufficient acetone ca.