Chloroform → HCID 86620647, compound
Reaction equation
[CH3:1][C:2]([NH:4][CH2:5][CH2:6][C:7]1[CH:8]=[C:9]([NH:13][C:14](=[O:17])[O:15][CH3:16])[CH:10]=[CH:11][CH:12]=1)=O.C(Cl)(Cl)Cl.P(Cl)(Cl)(Cl)(Cl)Cl>O>[CH3:1][C:2]1[C:12]2[C:7](=[CH:8][C:9]([NH:13][C:14](=[O:17])[O:15][CH3:16])=[CH:10][CH:11]=2)[CH2:6][CH2:5][N:4]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of 4.13 g (17.5 mmol) methyl N-[3-(2-methylcarbonylamino-ethyl)phenyl]carbamate and 35 ml chloroform is slowly combined with 8.00 g (38.4 mmol) phosphorus pentachloride and the mixture is stirred for 16 h. Then the mixture is carefully poured into water and stirred for 45 min. It is extracted 3× with methylene chloride and then the aqueous phase is made basic with 4N NaOH. The crystals precipitated are suction filtered and dried.
Workup
- stirringstirred for 45 min
- extractionIt is extracted 3× with methylene chloride
- customThe crystals precipitated
- filtrationare suction filtered
- customdried
Sources & evidence
- ORD record
- ord-d1dceaa090734430a04f703030c28e61
- Source dataset
- uspto-grants-2010_10
- Patent number
- US07807693B2
Reaction notes
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