Ethanol → HCID 178524123, compound

HRID 58929

Reaction equation

HRID 58929 reaction equation
[OH:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[CH:9][CH:8]=[CH:7]2.[Cl-].[Hf+4:13].[Cl-].[Cl-].[Cl-].[OH2:17].N1CCCCC1.[CH2:24]([OH:26])C>>[OH:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([C:24]([O-:26])=[O:17])[CH:8]=[CH:7]2.[OH:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([C:24]([O-:26])=[O:17])[CH:8]=[CH:7]2.[OH:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([C:24]([O-:26])=[O:17])[CH:8]=[CH:7]2.[OH:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([C:24]([O-:26])=[O:17])[CH:8]=[CH:7]2.[Hf+4:13]

Participants

6

Reactant 5

HCID 702Ethanol2×HCID 962WaterHCID 19238-HydroxyquinolineHCID 8082PiperidineHCID 9927068Hafnium chloride (HfCl4) (6CI,8CI); Hafnium chloride; Hafnium tetrachloride; Hafnium(IV) chloride; Hafnium chloride (HfCl4), (T-4)-

Product 1

HCID 178524123HCID 178524123, compound

Procedure

To a solution of 8-Hydroxyquinoline (5.44 g, 37.5 mmol) in ethanol (200 mL, 95%) was added hafnium (IV) chloride (3.0 g, 9.37 mmol) in ethanol (100 mL), followed by a further 300 mL water. The pH of the solution was increased by dropwise addition of piperidine until a yellow precipitate forms. The resulting yellow precipitate was collected and washed with ethanol (100 mL, 95%), water (200 mL) and finally ethanol (100 mL, 95%). The sample was dried under vacuum at 80° C. until no further weight loss was detected. Sublimation (400° C., 10−6 Torr) yielded an analytical sample (4.5 g, 64%), m.p. 398° C.

Workup

  1. customThe resulting yellow precipitate was collected
  2. washwashed with ethanol (100 mL, 95%), water (200 mL) and finally ethanol (100 mL, 95%)
  3. customThe sample was dried under vacuum at 80° C. until no further weight loss
  4. customSublimation (400° C., 10−6 Torr) yielded an analytical sample (4.5 g, 64%), m.p. 398° C.

Sources & evidence

ORD record
ord-644951c6206f42fa8b2a98e7ef1e0ec4
Source dataset
uspto-grants-2016_09
Patent number
US09437828B2

Linked notes

Loading…