Phosphoric Acid → HCID 12422112, compound

HRID 1763418Notes

Reaction equation

HRID 1763418 reaction equation
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.P(=O)(O)(O)O.[Cl:20][C:21]1[CH:38]=[CH:37][C:24]([CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[CH2:32][CH2:33][C:34]([OH:36])=O)=[CH:23][CH:22]=1>>[Cl:20][C:21]1[CH:22]=[CH:23][C:24]([CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[C:28]3[C:27]=2[CH2:32][CH2:33][C:34]3=[O:36])=[CH:37][CH:38]=1

Participants

4

Reactant 3

HCID 1004Phosphoric AcidHCID 14812Phosphorus oxide (P4O10)HCID 12422108HCID 12422108, compound

Product 1

HCID 12422112HCID 12422112, compound

Procedure

To stirred polyphosphoric acid, prepared from 100 g. of phosphorus pentoxide and 70 ml. of phosphoric acid, 5.0 g. of 3-(o-(p-chlorobenzyl)phenyl)propionic acid is added. The mixture is stirred at 110°-120° C for 2 hours. Upon addition of ice-water, yellow crystals separate out. These crystals are collected by filtration, washed with water and dried. The crystals are purified by column chromatography (silica gel; eluted with a 40:1 mixture of benzene and ethyl acetate. The described procedure gives 4-(p-chlorobenzyl)indan-1-one as crystals melting at 87°-88° C.

Workup

  1. customprepared from 100 g
  2. customseparate out
  3. filtrationThese crystals are collected by filtration
  4. washwashed with water
  5. customdried
  6. customThe crystals are purified by column chromatography (silica gel
  7. washeluted with a 40:1 mixture of benzene and ethyl acetate

Sources & evidence

ORD record
ord-d42ee66315e444fca2ec0b3f52f689a0
Source dataset
uspto-grants-1978_09
Patent number
US04111997

Reaction notes

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