Hydrochloric Acid → HCID 131711177, compound

HRID 2419135Notes

Reaction equation

HRID 2419135 reaction equation
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[S:3][C:2]1=[N:10][CH2:11][CH2:12][CH2:13][N:14]([CH3:16])[CH3:15].[ClH:17]>C(OCC)C>[ClH:17].[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[S:3][C:2]1=[N:10][CH2:11][CH2:12][CH2:13][N:14]([CH3:15])[CH3:16]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 20313837HCID 20313837, compound

Product 1

HCID 131711177HCID 131711177, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

A solution of N'-(1,3-benzodithiol-2-ylidene)-N,N-dimethyl-1,3-propanediamine (3.0g, prepared as described in Example 17) in 100 ml of anhydrous diethyl ether is treated dropwise with ethereal hydrogen chloride until precipitation is completed. The resultant solid is collected by filtration under a nitrogen atmosphere, washed several times with anhydrous diethyl ether and recrystallized twice from acetonitrile. The recrystallized product is washed with anhydrous diethyl ether and dried at atmospheric pressure under a slow stream of nitrogen to yield 3.1g of the title compound, melting point 188°-190° C.

Workup

  1. filtrationThe resultant solid is collected by filtration under a nitrogen atmosphere
  2. washwashed several times with anhydrous diethyl ether
  3. customrecrystallized twice from acetonitrile
  4. washThe recrystallized product is washed with anhydrous diethyl ether
  5. customdried at atmospheric pressure under a slow stream of nitrogen

Sources & evidence

ORD record
ord-1a2567422204417493c6a261026acaa5
Source dataset
uspto-grants-1978_08
Patent number
US04104467

Reaction notes

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