Ammonium Hydroxide → HCID 12677800, compound

HRID 2419476Notes

Reaction equation

HRID 2419476 reaction equation
[O:1]=[C:2]1[CH:7]=[C:6]([C:8]([OH:10])=[O:9])O[C:4]2[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[S:13][CH2:14][C:3]1=2.[OH-].[NH4+:20]>>[O:1]=[C:2]1[CH:7]=[C:6]([C:8]([OH:10])=[O:9])[NH:20][C:4]2[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[S:13][CH2:14][C:3]1=2

Participants

3

Reactant 2

HCID 14923Ammonium HydroxideHCID 12677785HCID 12677785, compound

Product 1

HCID 12677800HCID 12677800, compound

Procedure

A solution of 4-oxo-4H,5H-[1]benzothiopyrano[4,3-b]pyran-2-carboxylic acid (3.0 g, 11.53 mmoles, described in Example 79) in concentrated ammonium hydroxide (50 ml) is heated on a steam bath for 2.5 hr., and evaporated under reduced pressure. The residue is dissolved in water (75 ml) and added to a mixture of concentrated hyrochloric acid (5 ml) and ice. The precipitate is collected, washed with 0.07 N hydrochloric acid, acetone and ether to give the title compound as light yellow crystals, m.p. 256°-257° C.

Workup

  1. custom, and evaporated under reduced pressure
  2. dissolutionThe residue is dissolved in water (75 ml)
  3. additionadded to a mixture of concentrated hyrochloric acid (5 ml) and ice
  4. customThe precipitate is collected
  5. washwashed with 0.07 N hydrochloric acid, acetone and ether

Sources & evidence

ORD record
ord-3b6eb6c368044fdbb6edbd998b0538e5
Source dataset
uspto-grants-1978_08
Patent number
US04105778

Reaction notes

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