Hydrochloric Acid → HCID 178503294, compound

HRID 2369208Notes

Reaction equation

HRID 2369208 reaction equation
[CH3:1][S:2][C:3](=[C:6]([C:9]#[N:10])[C:7]#[N:8])SC.[C:11]([CH2:13][C:14]([NH2:16])=[S:15])#[N:12].C(N(CC)CC)C.Cl>CN(C=O)C>[NH2:10][C:9]1[C:6]([C:7]#[N:8])=[C:3]([S:2][CH3:1])[C:13]([C:11]#[N:12])=[C:14]([SH:15])[N:16]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 992292-(Bis(methylsulfanyl)methylidene)propanedinitrileHCID 14162772-Cyanoethanethioamide

Product 1

HCID 178503294HCID 178503294, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

10 g (58.74 mmol) of [bis(methylthio)methylene]malononitrile and 6.5 g (64.61 mmol) of cyanothioacetamide are initially charged in 20 ml of DMF, and 16.4 ml (117.5 mmol) of triethylamine are added dropwise at room temperature. The mixture is stirred at room temperature for 8 h and allowed to stand for a further two days. The mixture is then added to 250 ml of 3 N hydrochloric acid. The resulting precipitate is filtered off with suction, washed with water and acetone and dried. This gives a yellow powder.

Workup

  1. waitto stand for a further two days
  2. filtrationThe resulting precipitate is filtered off with suction
  3. washwashed with water and acetone
  4. customdried
  5. customThis gives a yellow powder

Sources & evidence

ORD record
ord-86a2a6f7d98f48a8b582a400458d32f4
Source dataset
uspto-grants-2014_04
Patent number
US08703934B2

Reaction notes

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