Potassium Cyanide → HCID 73180951, compound

HRID 1589126Notes

Reaction equation

HRID 1589126 reaction equation
ClCl.[CH:3](=[N:10][OH:11])[CH:4]1[CH2:9][CH2:8][CH2:7][CH2:6][O:5]1.[C-:12]#[N:13].[K+]>CCOCC.C(Cl)Cl.CO>[N:10](=[C:3]([CH:4]1[CH2:9][CH2:8][CH2:7][CH2:6][O:5]1)[C:12]#[N:13])[OH:11]

Participants

7

Procedure

7.8 g of chlorine were passed into a cooled solution of 12.9 g of 2-formyltetrahydropyran oxime in 140 ml of ether at below 0° C. Thereafter, the volatile constituents of the reaction mixture were stripped off, the residue was taken up in 200 ml of methylene chloride, and the mixture was kept at room temperature for 24 hours. This liquid was then added dropwise to a suspension, cooled to 10°-15° C., of 6.8 g of potassium cyanide in 75 ml of methanol, and the mixture was stirred for a further 3 hours at room temperature. The precipitated potassium chloride was filtered off under suction, the filtrate was evaporated down, the residue was taken up in ether, the solution was washed three times with water and dried over magnesium sulfate, and the solvent was stripped off under 0.005 mbar and at 30° C. to give 11.3 g of α-oximino(tetrahydropyran-2-yl)-acetonitrile as a yellowish solid which melted from 45° C.

Workup

  1. additionThis liquid was then added dropwise to a suspension
  2. filtrationThe precipitated potassium chloride was filtered off under suction
  3. customthe filtrate was evaporated down
  4. washthe solution was washed three times with water
  5. dry with materialdried over magnesium sulfate
  6. customwas stripped off under 0.005 mbar and at 30° C.

Sources & evidence

ORD record
ord-c00b37eb73a54a349278299f7d2a347d
Source dataset
uspto-grants-1986_02
Patent number
US04568668

Reaction notes

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