Potassium Cyanide → HCID 10585357, compound
Reaction equation
[C-:1]#[N:2].[K+].[NH4+:4].[Cl-].[CH2:6]1[C@H:19]2[C@@H:10]([CH2:11][C:12]3[C:17]([CH2:18]2)=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH2:9][CH2:8][C:7]1=O>CO.O.C(Cl)Cl>[NH2:4][C:7]1([C:1]#[N:2])[CH2:8][CH2:9][C@H:10]2[C@@H:19]([CH2:18][C:17]3[C:12]([CH2:11]2)=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:6]1Participants
7
Reactant 3
Product 1
Reagents, catalysts & solvents 3
Procedure
410 mg of KCN (6.3 mmol) and 340 mg of NH4Cl (6.3 mmol) are added, in succession, to a solution, stirred vigorously and maintained under nitrogen, containing 1.25 g (6.2 mmol) of the compound obtained in Step 4 in 30 ml of MeOH and 15 ml of water. After stirring for 12 hours at 20° C., the solution is diluted in CH2Cl2 and extracted with CH2Cl2. The organic phase is washed with a saturated NaCl solution, dried over MgSO4 and evaporated. The residue is treated with 25 ml of a methanolic solution of ammonia (7N) and stirred in a closed system for 12 hours at 20° C. Evaporation under reduced pressure yields the title compound in pure form.
Workup
- temperaturemaintained under nitrogen
- stirringAfter stirring for 12 hours at 20° C.
- extractionextracted with CH2Cl2
- washThe organic phase is washed with a saturated NaCl solution
- dry with materialdried over MgSO4
- customevaporated
- additionThe residue is treated with 25 ml of a methanolic solution of ammonia (7N)
- stirringstirred in a closed system for 12 hours at 20° C
- customEvaporation under reduced pressure
Sources & evidence
- ORD record
- ord-0f05ea598a584799b1daebe784c44556
- Source dataset
- uspto-grants-2001_01
- Patent number
- US06172097B2
Reaction notes
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