Ibuprofen, (+-)- → HCID 86745308, compound

HRID 1461227Notes

Reaction equation

HRID 1461227 reaction equation
[OH:1][CH2:2][C@@H:3]([C@H:5]([C@@H:7]([C@@H:9]([CH2:11][OH:12])[OH:10])[OH:8])[OH:6])[OH:4].[OH:13][C:14]([CH:16]([C:18]1[CH:27]=[CH:26][C:21]([CH2:22][CH:23]([CH3:25])[CH3:24])=[CH:20][CH:19]=1)[CH3:17])=[O:15]>>[OH:15][C:14]([CH:16]([C:18]1[CH:19]=[CH:20][C:21]([CH2:22][CH:23]([CH3:24])[CH3:25])=[CH:26][CH:27]=1)[CH3:17])=[O:13].[OH:12][CH2:11][C@@H:9]([C@H:7]([C@@H:5]([C@@H:3]([CH2:2][OH:1])[OH:4])[OH:6])[OH:8])[OH:10]

Participants

3

Reactant 2

HCID 3672Ibuprofen, (+-)-2×HCID 5780Sorbitol

Product 1

HCID 86745308HCID 86745308, compound

Conditions

Temperature
75 °C

Procedure

950 parts of a sorbitol were heated in a stainless steel mixer to 110° and then slowly cooled under high speed agitation to 75° C. and maintained at that temperature. 50 parts of ibuprofen (mp 75°-77° C.) were added very slowly to the vortex to ensure a homogenous distribution. After mixing for 10 minutes, the melt containing 5% ibuprofen was transferred to a Sigma blade mixer and the temperature maintained at 74° C., while agitation continued for 20 minutes at a rotation speed of 30 r.p.m. until the mixture partially crystallized. The partially solidified mass was removed from the mixer and placed on a tray to allow it to crystallize fully while held at a temperature of 50° C. for 12 hours. The material was cooled and ground and screened to produce a particle size distribution of -40/+100.

Workup

  1. custommixer to 110°
  2. temperaturemaintained at that temperature
  3. additionAfter mixing for 10 minutes
  4. temperaturethe temperature maintained at 74° C., while agitation
  5. customuntil the mixture partially crystallized
  6. customThe partially solidified mass was removed from the mixer
  7. customto crystallize fully
  8. temperatureThe material was cooled
  9. customto produce a particle size distribution of -40/+100

Sources & evidence

ORD record
ord-204769a0671b4989bed7237145f7db3d
Source dataset
uspto-grants-1991_12
Patent number
US05075291

Reaction notes

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