Hydrochloric Acid → HCID 15009007, compound

HRID 981068Notes

Reaction equation

HRID 981068 reaction equation
Cl.[S:2]([CH2:5][C:6]([CH2:8][S:9][C:10]#[N:11])=O)[C:3]#[N:4].C[OH:13]>>[S:2]([CH2:5][C:6]1[NH:11][C:10](=[O:13])[S:9][CH:8]=1)[C:3]#[N:4]

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 15009006HCID 15009006, compound

Product 1

HCID 15009007HCID 15009007, compoundYield 48.3%

Procedure

After absorbing 7.3 g (0.20 mol) of gaseous hydrogen chloride in 100 ml of anhydrous methanol, 17.22 g (0.10 mol) of 1,3-bis(thiocyanato)-acetone are added and the mixture is stirred at 45° to 50° C. for 4 hours. Then, the reaction mixture is evaporated under reduced pressure until a crystalline precipitate begins to separate. After cooling down the residue, the precipitate is filtered off. After washing with methanol and drying, 8.3 g (48.3%) of the named compound are obtained with the same quality characteristics as described in Example (1a). The active ingredient content of the substance obtained is 99.0%.

Workup

  1. additionare added
  2. customThen, the reaction mixture is evaporated under reduced pressure until a crystalline precipitate
  3. customto separate
  4. temperatureAfter cooling down the residue
  5. filtrationthe precipitate is filtered off
  6. washAfter washing with methanol
  7. customdrying

Sources & evidence

ORD record
ord-5ff9f7cae2d94f09a73b68c75801ebb3
Source dataset
uspto-grants-1991_02
Patent number
US04990524

Reaction notes

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