Ammonium Hydroxide → HCID 67089595, compound

HRID 2075392Notes

Reaction equation

HRID 2075392 reaction equation
[F:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][C:8]([C:12]([NH:14][NH:15][C:16]([NH2:18])=[S:17])=O)=[CH:7][CH:6]=2.[OH-].[NH4+]>S(=O)(=O)(O)O>[F:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][C:8]([C:12]1[S:17][C:16]([NH2:18])=[N:15][N:14]=1)=[CH:7][CH:6]=2

Participants

4

Reactant 2

HCID 14923Ammonium HydroxideHCID 86636675HCID 86636675, compound

Product 1

HCID 67089595HCID 67089595, compoundYield 92%

Reagents, catalysts & solvents 1

HCID 1118Sulfuric AcidSolvent

Procedure

A mixture of 1-(3-fluoroisoquinoline-6-carbonyl)thiosemicarbazide (0.98 g, 3.71 mmol) in sulfuric acid (10 mL) was stirred at room temperature for 3 hours. The mixture was poured into ice-ammonium hydroxide (33%). The pH was adjusted to >9 with additional ammonium hydroxide. The precipitate was recovered by filtration and washed with water (4×) to provide the product as an off-white solid (0.84 g, 92%). LCMS (API-ES) m/z: 247 (M+H+).

Workup

  1. filtrationThe precipitate was recovered by filtration
  2. washwashed with water (4×)

Sources & evidence

ORD record
ord-9f61a7c4cbd9448e9386f9014152e54e
Source dataset
uspto-grants-2011_04
Patent number
US07919504B2

Reaction notes

Loading…