Phosphorus oxychloride → HCID 14620586, compound
Reaction equation
[CH3:1][O:2][C:3](=[O:28])[CH2:4][C:5]1[C:13]([CH2:14][C:15]([NH:17][CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([O:26][CH3:27])[CH:21]=2)=O)=[CH:12][C:8]2[O:9][CH2:10][O:11][C:7]=2[CH:6]=1.P(Cl)(Cl)(Cl)=O>>[CH3:1][O:2][C:3](=[O:28])[CH2:4][C:5]1[C:13]([CH2:14][C:15]2[C:25]3[C:20](=[CH:21][C:22]([O:26][CH3:27])=[CH:23][CH:24]=3)[CH2:19][CH2:18][N:17]=2)=[CH:12][C:8]2[O:9][CH2:10][O:11][C:7]=2[CH:6]=1Participants
3
Procedure
The title compound was prepared as described in Example 7 using 6-[2-[[2-(3-methoxyphenyl)ethyl]amino]-2-oxoethyl]-1,3-benzodioxole-5-acetic acid methyl ester (VIIIb) (7.71 g, 0.02 mole) and phosphorus oxychloride (7.66 g, 0.05 mole). The crystalline product that was obtained was recrystallized from acetonitrile. The product was amounted to 1.4 g (15%), and melted at 182°-184° dec.
Workup
- customThe crystalline product that was obtained
- customwas recrystallized from acetonitrile
Sources & evidence
- ORD record
- ord-37c83497c7fc4896849d04903864d10f
- Source dataset
- uspto-grants-1989_07
- Patent number
- US04849420
Reaction notes
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