Water → HCID 131731758, compound

HRID 2403973Notes

Reaction equation

HRID 2403973 reaction equation
Cl.[N:2]1[CH:3]=[N:4][N:5]2[CH:10]=[C:9]([C:11]3[CH:20]=[C:19]4[C:14]([C@H:15]([C:21]5[CH:26]=[CH:25][C:24]([Cl:27])=[C:23]([Cl:28])[CH:22]=5)[CH2:16][NH:17][CH2:18]4)=[CH:13][CH:12]=3)[CH:8]=[CH:7][C:6]=12.[OH2:29]>C(O)(C)C>[OH2:29].[CH:7]([O-:29])([CH3:8])[CH3:6].[ClH:27].[N:2]1[CH:3]=[N:4][N:5]2[CH:10]=[C:9]([C:11]3[CH:20]=[C:19]4[C:14]([C@H:15]([C:21]5[CH:26]=[CH:25][C:24]([Cl:27])=[C:23]([Cl:28])[CH:22]=5)[CH2:16][NH:17][CH2:18]4)=[CH:13][CH:12]=3)[CH:8]=[CH:7][C:6]=12

Participants

4

Reactant 2

HCID 962WaterHCID 66788517HCID 66788517, compound

Product 1

HCID 131731758HCID 131731758, compound

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Procedure

(S)-7-([1,2,4]triazolo[1,5-a]pyridin-6-yl)-4-(3,4-dichlorophenyl)-1,2,3,4-tetrahydroisoquinoline mono-HCl salt (20 mg) was dissolved in isopropanol (10 mL) under heating in a vial. Distilled water (2 mL) was then added to the above clear solution. The resulting solution was capped and placed at room temperature. Long needle crystals of (S)-7-([1,2,4]triazolo[1,5-a]pyridin-6-yl)-4-(3,4-dichlorophenyl)-1,2,3,4-tetrahydroisoquinoline mono-HCl monoisopropanolate monohydrate salt were obtained after slow evaporation in air within days. The needle-like crystals were separated from mother liquor by filtration and the wet cake was dried in an oven for 16 hours under the condition of 45° C. and 100 mmHg.

Workup

  1. temperatureunder heating in a vial
  2. customThe resulting solution was capped
  3. customplaced at room temperature

Sources & evidence

ORD record
ord-2a465eb1651e4415ae12061d1f8eb89b
Source dataset
uspto-grants-2014_08
Patent number
US08802696B2

Reaction notes

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