Water → HCID 22117217, compound

HRID 1275910Notes

Reaction equation

HRID 1275910 reaction equation
[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][CH2:9][C:10]2[CH:18]=[C:17]([C:19]([F:22])([F:21])[F:20])[CH:16]=[CH:15][C:11]=2[C:12]([OH:14])=O)[CH:5]=[CH:6][CH:7]=1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.O>[N+](C1C=CC=CC=1)([O-])=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]2[C:12](=[O:14])[C:11]3[CH:15]=[CH:16][C:17]([C:19]([F:22])([F:21])[F:20])=[CH:18][C:10]=3[CH2:9][CH2:8][C:4]=2[CH:3]=1

Participants

5

Reactant 3

HCID 962WaterHCID 14812Phosphorus oxide (P4O10)HCID 22117183HCID 22117183, compound

Product 1

HCID 22117217HCID 22117217, compound

Reagents, catalysts & solvents 1

HCID 7416NitrobenzeneSolvent

Conditions

Temperature
100 °C

Procedure

A mixture of the product from step (iv) (2.31 g) and phosphorous pentoxide (14 g) in nitrobenzene (15 ml) was heated at 100° C. for 8 hours. The solid mixture was added to water, salted out and extracted with ethyl acetate. The extract was dried (MgSO4) and evaporated, distilled to remove nitrobenzene and the residue purified by chromatography eluting with 10% ethyl acetate in isohexane. Yield 1.14 g.

Workup

  1. extractionextracted with ethyl acetate
  2. dry with materialThe extract was dried (MgSO4)
  3. customevaporated
  4. distillationdistilled
  5. customto remove nitrobenzene
  6. customthe residue purified by chromatography
  7. washeluting with 10% ethyl acetate in isohexane

Sources & evidence

ORD record
ord-878295d4d8864cf2b211593c3206e3dd
Source dataset
uspto-grants-2000_12
Patent number
US06162808

Reaction notes

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