Ammonia → HCID 59134442, compound

HRID 1993648Notes

Reaction equation

HRID 1993648 reaction equation
S(S([O-])=O)([O-])=O.[Na+].[Na+].[Cl:9][C:10]1[C:15]([N+:16]([O-])=O)=[CH:14][N:13]=[C:12]([N:19]2[CH2:24][CH2:23][N:22]([C:25](=[O:30])[C:26]([CH3:29])([CH3:28])[CH3:27])[CH2:21][CH2:20]2)[CH:11]=1.O1CCCC1.N>O>[NH2:16][C:15]1[C:10]([Cl:9])=[CH:11][C:12]([N:19]2[CH2:24][CH2:23][N:22]([C:25](=[O:30])[C:26]([CH3:27])([CH3:28])[CH3:29])[CH2:21][CH2:20]2)=[N:13][CH:14]=1

Participants

6

Reactant 4

HCID 222AmmoniaHCID 8028TetrahydrofuranHCID 24489Sodium DithioniteHCID 68541591HCID 68541591, compound

Product 1

HCID 59134442HCID 59134442, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Add (4.5 mmol, 0.8 g) of sodium dithionite, over 1-[4-(4-chloro-5-nitro-pyridin-2-yl)-piperazin-1-yl]-2,2-dimethyl-propan-1-one (0.9 mmol, 0.3 g) in 22 mL of 1:1 mixture of tetrahydrofuran and water and 4 mL of ammonia. Stir the solution for 2 hours at room temperature. Concentrate under reduce pressure and extract the residue in ethyl acetate. Dry over sodium sulfate, filter, and concentrate under reduced pressure to give a residue that is used without further purification. MS(ES): m/z=297 [M+H].

Workup

  1. concentrationConcentrate
  2. extractionextract the residue in ethyl acetate
  3. dry with materialDry over sodium sulfate
  4. filtrationfilter
  5. concentrationconcentrate under reduced pressure
  6. customto give a residue that
  7. customis used without further purification

Sources & evidence

ORD record
ord-4a1e2213101741b1a26d589b5f850330
Source dataset
uspto-grants-2010_01
Patent number
US07652015B2

Reaction notes

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