Chloroform → 156122-75-7

HRID 1509772Notes

Reaction equation

HRID 1509772 reaction equation
C[O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[N:14]=[C:13]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[O:27]C)[N:16]=2)[CH:12]=[CH:11][CH:10]=1.Cl.N1C=CC=CC=1.C(Cl)(Cl)Cl>O>[OH:27][C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=1[C:17]1[N:16]=[C:15]([C:13]2[CH:12]=[CH:11][CH:10]=[C:9]([C:4]3[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=3[OH:2])[N:14]=2)[CH:20]=[CH:19][CH:18]=1

Participants

5

Reactant 3

HCID 6212ChloroformHCID 10176127Pyridinium chlorideHCID 23110539HCID 23110539, compound

Product 1

HCID 135430854156122-75-7Yield 72.2%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
160 °C

Procedure

A mixture of a 6,6′-bis(2-methoxyphenyl)-2,2′-bipyridyl ligand (0.3 g) and pyridine hydrochloride (10 g) was heated for 4 hours at 160° C. under a nitrogen atmosphere. After cooling the reaction solution to a room temperature, chloroform (20 ml) and water (20 ml) were added to the reaction solution for separation. Thereafter, the organic layer was concentrated. Purification by silica gel chromatography (chloroform as a developing solvent) was carried out, to obtain 0.2 g of 6,6′-bis(2-hydroxyphenyl)-2,2′-bipyridyl.

Workup

  1. temperatureAfter cooling the reaction solution to a room temperature
  2. concentrationThereafter, the organic layer was concentrated
  3. customPurification by silica gel chromatography (chloroform as a developing solvent)

Sources & evidence

ORD record
ord-66cccb7d217f48faa7236c6d13fc562d
Source dataset
uspto-grants-2012_07
Patent number
US08211553B2

Reaction notes

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