Water → HCID 12052173, compound

HRID 1018929Notes

Reaction equation

HRID 1018929 reaction equation
[CH2:1]([S:8][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[N:11][N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH:25]OS([O-])=O.[K+].OS([O-])(=O)=O.[K+].[OH2:37]>CN(C)C(=O)C>[CH2:1]([S:8]([C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[N:11][N:10]=1)(=[O:25])=[O:37])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

6

Procedure

1-Benzylthio-4-phenylphthalazine (98 mg; 0.3 mmol from Example 1B) in N,N-dimethylacetamide (13 ml) is cooled in an ice bath. Oxone® (2KHSO5.KHSO4.K2SO4) (670 mg; 1.1 mmol) is added, followed by the stepwise addition of water (1.4 ml). The mixture is stirred at room temperature for 2 days, is poured into ice water, is stirred 10 minutes and is filtered to give the title compound as a solid (53 mg) (R1=phenyl, R2=phenyl, A=benzene, Y1=CH2, m=0, n=1, p=0, q=2).

Workup

  1. stirringis stirred 10 minutes
  2. filtrationis filtered

Sources & evidence

ORD record
ord-02246dd1c8644baa8f8b9b020087e569
Source dataset
uspto-grants-2002_11
Patent number
US06486158B1

Reaction notes

Loading…