Hydrochloric Acid → HCID 69447876, compound

HRID 2060072Notes

Reaction equation

HRID 2060072 reaction equation
[ClH:1].Cl.[CH3:3][N:4]([CH2:6][CH:7]1[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[C:12]([O:16][C:17]([F:20])([F:19])[F:18])[CH:13]=2)[C:8]1([C:22]1[CH:23]=[N:24][CH:25]=[CH:26][CH:27]=1)O)[CH3:5]>CC(C)=O>[ClH:1].[CH3:3][N:4]([CH3:5])[CH2:6][C:7]1[CH2:15][C:14]2[C:9]([C:8]=1[C:22]1[CH:23]=[N:24][CH:25]=[CH:26][CH:27]=1)=[CH:10][CH:11]=[C:12]([O:16][C:17]([F:20])([F:18])[F:19])[CH:13]=2

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 69447481HCID 69447481, compound

Product 1

HCID 69447876HCID 69447876, compound

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

About 10.8 ml of 37% hydrochloric acid were added at room temperature to 1.2 g of 2-dimethylaminomethyl-1-pyridin-3-yl-5-trifluoromethoxy-indan-1-ol hydrochloride (mixture of the diastereoisomers), and stirring was carried out overnight; 15 ml of acetone p.a. were added, and stirring was carried out for 2 hours. An oily, semi-crystalline precipitate formed, from which the supernatant was separated off. The residue was taken up in about 40 ml of acetone p.a. and stirred, whereupon fine crystals formed, which were filtered off with suction, with the exclusion of air, washed twice with diethyl ether and dried under an oil-pump vacuum at from 25 to 60° C. 1.17 g of dimethyl-(3-pyridin-3-yl-6-trifluoromethoxy-1H-inden-2-ylmethyl)-amine hydrochloride were obtained.

Workup

  1. additionmixture of the diastereoisomers), and
  2. additionwere added
  3. stirringstirring
  4. waitwas carried out for 2 hours
  5. customAn oily, semi-crystalline precipitate formed, from which the supernatant
  6. customwas separated off
  7. stirringand stirred, whereupon fine crystals
  8. customformed
  9. filtrationwhich were filtered off with suction, with the exclusion of air
  10. washwashed twice with diethyl ether
  11. customdried under an oil-pump vacuum at from 25 to 60° C

Sources & evidence

ORD record
ord-ce9456d2a0db45b2814cb86f669704f8
Source dataset
uspto-grants-2012_10
Patent number
US08278338B2

Reaction notes

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