Hydrochloric Acid → Lesopitron dihydrochloride

HRID 362778Notes

Reaction equation

HRID 362778 reaction equation
[CH:1]1[CH:2]=[N:3][C:4]([N:7]2[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][N:17]3[N:21]=[CH:20][C:19]([Cl:22])=[CH:18]3)[CH2:9][CH2:8]2)=[N:5][CH:6]=1.[ClH:23]>C(O)(C)C>[CH2:9]1[N:10]([CH2:13][CH2:14][CH2:15][CH2:16][N:17]2[N:21]=[CH:20][C:19]([Cl:22])=[CH:18]2)[CH2:11][CH2:12][N:7]([C:4]2[N:3]=[CH:2][CH:1]=[CH:6][N:5]=2)[CH2:8]1.[ClH:23].[ClH:22]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 60813Lesopitron

Product 1

HCID 60812Lesopitron dihydrochlorideYield 195.5%

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Procedure

A 250 L enamelled reactor was loaded with an isopropanolic solution (57 Kg) of Lesopitron (25.2 mol), and was cooled to 5°-10° C. Subsequently, 8.5 Kg of a solution of hydrochloric acid (58.3 mol) in isopropanol were added, keeping the temperature between 5° and 15° C. during the addition. After stirring the suspension for 30 minutes, the product was centrifuged and washed with isopropanol. The Lesopitron dihydrochloride was washed and then dried in an air oven at 40° C. for 15 hours, obtaining 9.7 Kg (98% yield) of the compound mentioned in the title.

Workup

  1. temperaturewas cooled to 5°-10° C
  2. customthe temperature between 5° and 15° C.
  3. additionduring the addition
  4. washwashed with isopropanol
  5. washThe Lesopitron dihydrochloride was washed
  6. customdried in an air oven at 40° C. for 15 hours

Sources & evidence

ORD record
ord-57d25957bbf443e6b00767cf1aa41038
Source dataset
uspto-grants-1999_02
Patent number
US05872125

Reaction notes

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