Hydrochloric Acid → 107007-99-8

HRID 215980Notes

Reaction equation

HRID 215980 reaction equation
[CH3:1][N:2]1[N:10]=[C:9]([C:11]([NH:13][CH:14]2[CH2:21][CH:20]3[N:22]([CH3:23])[CH:16]([CH2:17][CH2:18][CH2:19]3)[CH2:15]2)=[O:12])[C:8]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]1=2.[ClH:24]>C1(C)C=CC=CC=1>[CH3:1][N:2]1[N:10]=[C:9]([C:11]([NH:13][CH:14]2[CH2:21][CH:20]3[N:22]([CH3:23])[CH:16]([CH2:17][CH2:18][CH2:19]3)[CH2:15]2)=[O:12])[C:8]2[CH:7]=[CH:6][CH:5]=[CH:4][C:3]1=2.[ClH:24]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 35101-Methyl-N-(9-methyl-9-azabicyclo[3.3.1]nonan-3-yl)-1H-indazole-3-carboxamide

Product 1

HCID 65264107007-99-8

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
55 °C

Procedure

Granisetron (60.0 g) and toluene (12 parts) are charged to a suitable reactor and heated to dissolution. Conc. hydrochloric acid (1.1 eq) is added drop wise while maintaining the temperature at 50 to 60° C. The resulting suspension is distilled at below 80° C. to ⅔ volume and cooled to below 10° C. The solid is collected and dried to provide granisetron hydrochloride (53.6-67 g).

Workup

  1. temperatureheated to dissolution
  2. distillationThe resulting suspension is distilled at below 80° C.
  3. temperaturecooled to below 10° C
  4. customThe solid is collected
  5. customdried

Sources & evidence

ORD record
ord-ea0fa1e3490d4219a94332c92fa087fa
Source dataset
uspto-grants-2012_06
Patent number
US08193217B2

Reaction notes

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