Phosphorus oxychloride → HCID 86636835, compound
Reaction equation
[CH3:1][O:2][C:3]([C:5]1[C:10]2[C:11]3[C:12](O)=[N:13][CH:14]=[CH:15][C:16]=3[O:17][C:9]=2[C:8]([O:19]C2CCCC2)=[CH:7][CH:6]=1)=[O:4].P(Cl)(Cl)([Cl:27])=O>>[CH3:1][O:2][C:3]([C:5]1[C:10]2[C:11]3[C:12]([Cl:27])=[N:13][CH:14]=[CH:15][C:16]=3[O:17][C:9]=2[C:8]([OH:19])=[CH:7][CH:6]=1)=[O:4]Participants
3
Procedure
A solution of Methyl-1-hydroxy-6-cyclopentyloxybenzo[4,5]furo[3,2-c]pyridine-9-carboxylate (16.0 g) and phosphorous oxychloride (320 mL) was refluxed for 15-16 hours. Phosphorous oxychloride (300 mL) was removed under vacuo. Water (20.0 ml) was added at 60-70° C. Then after water (200 mL) was added, the solid obtained was filtered, washed with water (2×100 mL) and dried to get 8.8 g of product as yellow solid.
Workup
- customPhosphorous oxychloride (300 mL) was removed under vacuo
- additionWater (20.0 ml) was added at 60-70° C
- additionThen after water (200 mL) was added
- customthe solid obtained
- filtrationwas filtered
- washwashed with water (2×100 mL)
- customdried
Sources & evidence
- ORD record
- ord-0f953c00e4a64857b8e4ca31245b370c
- Source dataset
- uspto-grants-2012_03
- Patent number
- US08129401B2
Reaction notes
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