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温度

0 °C

A solution of 1,3-diaminocyclohexane (1.14 g, 10 mmol, undetermined isomer mixture) in methylene chloride (50 mL) was cooled to 0° C. and phenylsulfonyl chloride (0.64 mL, 5 mmol) was added dropwise. The mixture was stirred at 0° C. for 4 h, then 1N sodium hydroxide solution (10 mL) was added and the mixture stirred an additional 5 min. The phases were separated, the organic phase was dried (K2CO3), filtered, and concentrated in vacuo. Toluene was added and the mixture re-concentrated to remove any remaining diamine, to give 0.77 g of a semi solid. 1H—NMR was consistent with the desired structure. MS (ion spray) 255 (M+1).

1. stirringthe mixture stirred an additional 5 min
2. customThe phases were separated
3. dry with materialthe organic phase was dried (K2CO3)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. additionToluene was added
7. concentrationthe mixture re-concentrated
8. customto remove any remaining diamine
9. customto give 0.77 g of a semi solid