Ammonia → HCID 16793423, compound

HRID 1733144Notes

Reaction equation

HRID 1733144 reaction equation
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:6]=1[C:7]#[N:8].S(=O)(=O)(O)[OH:14].N>>[NH2:1][C:2]1[S:3][CH:4]=[C:5]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:6]=1[C:7]([NH2:8])=[O:14]

Participants

4

Reactant 3

HCID 222AmmoniaHCID 1118Sulfuric AcidHCID 5968662-Amino-4-(1,1-dimethylethyl)-3-thiophenecarbonitrile

Product 1

HCID 16793423HCID 16793423, compound

Procedure

A mixture of 180 g (1 mole) of 2-amino-3-cyano-4-tert.-butyl-thiophene and 750 ml of 95-97% strength sulphuric acid was stirred at 100°-110° C. for one hour, whereupon a slightly exothermic reaction started, so that when a temperature of 100° C. was reached no further heating was required. The reaction mixture was left to cool and was stirred into 5 liters of ice-water and neutralized with about 3 liters of 25% strength aqueous ammonia solution. The solid product which precipitated was filtered off, washed with water and dried at 50° C. 194 g of 2-amino-3-aminocarbonyl-4-tert.-butyl-thiophene of melting point 145° C. were obtained in this manner.

Workup

  1. customa temperature of 100° C.
  2. temperatureno further heating
  3. waitThe reaction mixture was left
  4. temperatureto cool
  5. customThe solid product which precipitated
  6. filtrationwas filtered off
  7. washwashed with water
  8. customdried at 50° C

Sources & evidence

ORD record
ord-2b7ce72ab2a342b0872800beb23b9860
Source dataset
uspto-grants-1980_12
Patent number
US04240820

Reaction notes

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