Ethanol → HCID 22484390, compound

HRID 1076948Notes

Reaction equation

HRID 1076948 reaction equation
C([OH:3])C.[C:4]([OH:13])(=[O:12])[C@@H:5]([C@H:7]([C:9]([OH:11])=[O:10])[OH:8])[OH:6]>O>[C:9]([CH:7]([CH:5]([C:4]([O-:13])=[O:12])[OH:6])[OH:8])([O-:11])=[O:10].[OH2:3]

Participants

4

Reactant 2

HCID 702EthanolHCID 444305L-Tartaric acid

Product 1

HCID 22484390HCID 22484390, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
70 °C

Procedure

In 50 volume parts of water are dissolved 19 parts of TRH monohydrate and 7.5 parts of L-tartaric acid, and while the solution is warmed to 70°C, ethanol is added in installments. Immediately after a slight turbidity is observed, the temperature is gradually brought down to room temperature, at which temperature the solution is allowed to stand for 3 days. Then, the solution is cooled to 10°C and allowed to stand for 2 days to allow crystallization to be completed. The crystals thus obtained are harvested by filtration, washed with hot ethanol and dried under reduced pressure at 50°C for 1 hour and at 80°C for 5 hours. The described procedure yields 18 parts of TRH tartrate-water as crystals melting at 127°C-130°C. [α]D 24 =-49.90°(c=1.05 in water)

Workup

  1. customis gradually brought down to room temperature, at which temperature
  2. temperatureThen, the solution is cooled to 10°C
  3. waitto stand for 2 days
  4. customcrystallization
  5. customThe crystals thus obtained
  6. filtrationare harvested by filtration
  7. washwashed with hot ethanol
  8. customdried under reduced pressure at 50°C for 1 hour and at 80°C for 5 hours

Sources & evidence

ORD record
ord-eedcaefb63484f2e9f309f332ee527fd
Source dataset
uspto-grants-1976_05
Patent number
US03959247

Reaction notes

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