Water → HCID 12073437, compound

HRID 2058949Notes

Reaction equation

HRID 2058949 reaction equation
[C:1]([C:3]1[C:12](=[O:13])[C:11]2[C:6](=[C:7]([Cl:15])[CH:8]=[C:9]([Cl:14])[CH:10]=2)[O:5][CH:4]=1)#N.N([O-])=[O:17].[Na+].[OH2:20]>S(=O)(=O)(O)O>[Cl:14][C:9]1[CH:10]=[C:11]2[C:6](=[C:7]([Cl:15])[CH:8]=1)[O:20][CH:1]=[C:3]([C:4]([OH:17])=[O:5])[C:12]2=[O:13]

Participants

5

Reactant 3

HCID 962Water2×HCID 7360206,8-Dichloro-3-cyanochromoneHCID 23668193Sodium Nitrite

Product 1

HCID 12073437HCID 12073437, compound

Reagents, catalysts & solvents 1

HCID 1118Sulfuric AcidSolvent2×

Procedure

8 g of the product of step (a) are dissolved in 30 ml of conc. sulphuric acid and the solution is allowed to stand for 18 hours at room temperature. After addition of 90 m of conc. and 200 ml of 80% sulphuric acid, 5.5 g of sodium nitrite in 10 ml of water are introduced under the liquid surface at 5°-10°. The mixture is stirred at 10° for 15 minutes and at 70° for 30 minutes and then poured into 1 l of water. The resulting precipitate is separated, washed 3 times with water and twice with ethanol, to obtain the heading compound, m.p. 196°, which can be crystallised from acetic acid.

Workup

  1. additionare introduced under the liquid surface at 5°-10°
  2. customThe resulting precipitate is separated
  3. washwashed 3 times with water
  4. customtwice with ethanol, to obtain the heading compound, m.p. 196°, which
  5. customcan be crystallised from acetic acid

Sources & evidence

ORD record
ord-dfc7338a7bf04c048139b5ce446b1a9c
Source dataset
uspto-grants-1982_03
Patent number
US04320133

Reaction notes

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