Sorbitol → HCID 178485001, compound

HRID 1461226Notes

Reaction equation

HRID 1461226 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].[CH3:13][C:14]1[NH:18][CH:17]=[N:16][C:15]=1[CH2:19][S:20][CH2:21][CH2:22]/[N:23]=[C:24](/[NH:27][C:28]#[N:29])\[NH:25][CH3:26]>O>[CH3:13][C:14]1[NH:18][CH:17]=[N:16][C:15]=1[CH2:19][S:20][CH2:21][CH2:22]/[N:23]=[C:24](/[NH:27][C:28]#[N:29])\[NH:25][CH3:26].[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

4

Reactant 2

HCID 5780Sorbitol3×HCID 178484997HCID 178484997, compound

Product 1

HCID 178485001HCID 178485001, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
105 °C

Procedure

474 parts of anhydrous sorbitol were melted in a stainless steel reactor equipped with agitation means and heated to a temperature of 105° C. The molten sorbitol was agitated at a speed of 100 r.p.m. to create a vortex and thereafter 25 parts of cimetidine (melting point 141°-143° C.) were added to the vortex slowly to avoid forming lumps. After complete addition, the melt was agitated for an additional 10 minutes. This melt was transferred to a Sigma blade mixer heated at 90° C. with hot water and agitated at 18 r.p.m. After 1 minute of mixing, 1% crystalline sorbitol seed fines (less than 325 mesh) were slowly added over the surface of the agitating melt to achieve a uniform dispersion of the seeds in the melt in order to initiate a rapid crystallization in the mixer. When the crystallizing mass achieved a dough-like consistency in the mixer, it was removed and placed on a tray, spread out and placed in an oven at 50° C. for 10 hours until it was fully crystallized. The crystalline mass was cooled and aggregates of the material were ground in a laboratory Waring blender (medium speed, 5 seconds), then screened to collect a -40/+100 mesh fraction.

Workup

  1. customequipped with agitation means
  2. customto avoid forming lumps
  3. additionAfter complete addition
  4. stirringagitated at 18 r.p.m
  5. additionAfter 1 minute of mixing
  6. customa rapid crystallization in the mixer
  7. customwas removed
  8. waitplaced in an oven at 50° C. for 10 hours until it
  9. customwas fully crystallized
  10. temperatureThe crystalline mass was cooled
  11. customwere ground in a laboratory Waring blender (medium speed, 5 seconds)
  12. customto collect a -40/+100 mesh fraction

Sources & evidence

ORD record
ord-da296d10991d4262a9c782b1f25ed4ae
Source dataset
uspto-grants-1991_12
Patent number
US05075291

Reaction notes

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