Acetonitrile → HCID 86733458, compound

HRID 1076950Notes

Reaction equation

HRID 1076950 reaction equation
[C:1](#[N:3])[CH3:2].[C:4]([OH:13])(=[O:12])[C@@H:5]([C@H:7]([C:9]([OH:11])=[O:10])[OH:8])[OH:6]>C(O)(=O)C>[C:9]([CH:7]([CH:5]([C:4]([O-:13])=[O:12])[OH:6])[OH:8])([O-:11])=[O:10].[C:1](#[N:3])[CH3:2]

Participants

4

Reactant 2

HCID 6342AcetonitrileHCID 444305L-Tartaric acid

Product 1

HCID 86733458HCID 86733458, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Conditions

Temperature
50 °C

Procedure

In 80 volume parts of acetic acid are dissolved 19 parts of TRH monohydrate and 7.5 parts of L-tartaric acid, and while the solution is warmed to 50°C, 240 volume parts of acetonitrile is added in installments. The temperature is gradually brought down to room temperature, at which temperature the solution is allowed to stand overnight. The resultant crystals are harvested by filtration, washed with acetonitrile and dried under reduced pressure. The procedure yields 25.7 parts of TRH tartrate-acetonitrile as crystals melting at 145°C-148°C. [α]D22 =-47.1° (c=1.0 in water)

Workup

  1. customis gradually brought down to room temperature, at which temperature
  2. filtrationThe resultant crystals are harvested by filtration
  3. washwashed with acetonitrile
  4. customdried under reduced pressure

Sources & evidence

ORD record
ord-9fa1b05e664c4e59b7db0d31a0cfd99b
Source dataset
uspto-grants-1976_05
Patent number
US03959247

Reaction notes

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