Dichloromethane → HCID 67263440, compound
Reaction equation
P(Cl)(Cl)(Cl)(Cl)Cl.[N+:7]([C:10]1[CH:20]=[CH:19][C:13]([O:14][CH2:15][C:16](O)=[O:17])=[C:12]([N:21]2[CH:25]=[CH:24][CH:23]=[CH:22]2)[CH:11]=1)([O-:9])=[O:8].C(Cl)Cl.[OH-].[Na+]>>[N+:7]([C:10]1[CH:20]=[CH:19][C:13]2[O:14][CH2:15][C:16](=[O:17])[C:25]3[N:21]([CH:22]=[CH:23][CH:24]=3)[C:12]=2[CH:11]=1)([O-:9])=[O:8]Participants
5
Procedure
PCl5 (1.30 g, 6.25 mmol) was added slowly to (4-Nitro-2-pyrrol-1-yl-phenoxy)-acetic acid (1.5 g, 5.7 m mol) in CH2Cl2 (40 mL, 0.6 mol) and the reaction mixture was stirred at rt for 16 h. The reaction mixture was poured onto crushed ice, basified with 1 N NaOH, and extracted with CH2Cl2. The organic layer was dried over MgSO4, filtered, and concentrated under reduced pressure. LCMS 245.10 (M+H).
Workup
- additionThe reaction mixture was poured
- customonto crushed ice
- extractionextracted with CH2Cl2
- dry with materialThe organic layer was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
Sources & evidence
- ORD record
- ord-705620ced206497a99c6998a1e298439
- Source dataset
- uspto-grants-2012_04
- Patent number
- US08148391B2
Reaction notes
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