反应详情

To an ice cold solution of tert-butyl 3-aminopropylcarbamate (3.56 g, 20.43 mmol) in CH2Cl2 (80 mL) is added dropwise benzoyl isothiocyanate (3.50 g, 21.45 mmol). The reaction mixture is stirred at room temp for 2 h after which the solvent is removed in vacuo. The resulting residue is partitioned with CH2Cl2 and water, the water layer is extracted with CH2Cl2, the organic layers are combined, washed with brine, dried over Na2SO4, filtered and evaporated to dryness to give 6.89 g (quantitative yield) of the title compound. LC/MS (Condition A): ret. T=3.56 min, (M+H)+ 338.26.

1. customis removed in vacuo
2. customThe resulting residue is partitioned with CH2Cl2 and water
3. extractionthe water layer is extracted with CH2Cl2
4. washwashed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customevaporated to dryness