Lactose monohydrate → (+)-Lactose

HRID 1248798Notes

Reaction equation

HRID 1248798 reaction equation
O.[OH:2][CH:3]1[O:22][C@H:21]([CH2:23][OH:24])[C@@H:8]([O:9][C@@H:10]2[O:18][C@H:17]([CH2:19][OH:20])[C@H:15]([OH:16])[C@H:13]([OH:14])[C@H:11]2[OH:12])[C@H:6]([OH:7])[C@H:4]1[OH:5]>O>[OH:2][CH:3]1[O:22][C@H:21]([CH2:23][OH:24])[C@@H:8]([O:9][C@@H:10]2[O:18][C@H:17]([CH2:19][OH:20])[C@H:15]([OH:16])[C@H:13]([OH:14])[C@H:11]2[OH:12])[C@H:6]([OH:7])[C@H:4]1[OH:5]

Participants

3

Reactant 1

HCID 62223Lactose monohydrate

Product 1

HCID 440995(+)-Lactose

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
-40 °C

Procedure

A solution of lactose monohydrate in water having a concentration of between about 5% and about 15% w/w is poured into stainless steel pans prechilled to about -35° C. The freeze dryer shelf temperature is maintained at -40° C. until the solution is frozen. The drying chamber is evacuated and primary drying is conducted at a temperature below -31.5° C. (pan contents). The temperature of the pan contents (frozen solution) is maintained at a temperature of between about -33° C. and about -38° C. by control of the shelf temperature at between about -15° C. and about -18° C. and a chamber pressure of between about 60 microns and 70 microns. When ice sublimation is complete as indicated by the temperature readings of the pan contents, secondary drying is conducted at a shelf temperature of about 25° C. for 15 h and at about 40° C. for 3 h. The amorphous lactose obtained has a water content of between about 1% and about 2%.

Workup

  1. customprechilled to about -35° C
  2. temperatureis frozen
  3. customThe drying chamber is evacuated
  4. customprimary drying
  5. customis conducted at a temperature below -31.5° C. (pan contents)
  6. temperatureThe temperature of the pan contents (frozen solution)
  7. temperatureis maintained at a temperature of between about -33° C. and about -38° C. by control of the shelf temperature at between about -15° C. and about -18° C.
  8. customsecondary drying

Sources & evidence

ORD record
ord-e13d0afa4fec4316ba7643c5944caebb
Source dataset
uspto-grants-1986_12
Patent number
US04626534

Reaction notes

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