Water → HCID 90088337, compound

HRID 2202136Notes

Reaction equation

HRID 2202136 reaction equation
[C:1]1([S:7]([O:10][C:11]2[CH:12]=[CH:13][CH:14]=[C:15]3[C:20]=2[O:19][C:18](=[O:21])[C:17]([NH:22]C(=O)C)=[CH:16]3)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(=O)(=O)(O)O.O>C(O)(=O)C>[C:1]1([S:7]([O:10][C:11]2[CH:12]=[CH:13][CH:14]=[C:15]3[C:20]=2[O:19][C:18](=[O:21])[C:17]([NH2:22])=[CH:16]3)(=[O:8])=[O:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

5

Reactant 3

HCID 962WaterHCID 1118Sulfuric AcidHCID 90088357HCID 90088357, compound

Product 1

HCID 90088337HCID 90088337, compoundYield 83.5%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Conditions

Temperature
50 °C

Procedure

To a solution of the compound produced in the above (1) (3.0 g, 8.3 mmol) in acetic acid (30 mL) was added 50 vol % sulfuric acid (30 mL) followed by stirring at 50° C. After the crystals were completely dissolved, the reaction mixture was allowed to cool and added to water. The crystals separated out therefrom were filtered and dried to give 2.2 g (83%) of the title compound.

Workup

  1. dissolutionAfter the crystals were completely dissolved
  2. temperatureto cool
  3. customThe crystals separated out
  4. filtrationtherefrom were filtered
  5. customdried

Sources & evidence

ORD record
ord-e3661e3ed04b4c3ca7e5ff402bd4e35e
Source dataset
uspto-grants-2016_06
Patent number
US09365533B2

Reaction notes

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