Perchloric Acid → HCID 14555943, compound

HRID 1164784Notes

Reaction equation

HRID 1164784 reaction equation
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[O:6][CH2:7][O:8][C:9]3[CH:22]=[CH:21][CH:20]=[CH:19][C:10]=3[N:11]([CH2:12][CH:13]([CH3:18])[CH2:14][N:15]([CH3:17])[CH3:16])[C:4]=2[CH:3]=1.Cl(O)(=O)(=O)=O.[C:30]([OH:39])(=[O:38])[C@@H:31]([C@H:33]([C:35]([OH:37])=[O:36])[OH:34])[OH:32]>ClCCl>[C:35]([C@@H:33]([C@H:31]([C:30]([OH:39])=[O:38])[OH:32])[OH:34])([OH:37])=[O:36].[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[O:6][CH2:7][O:8][C:9]3[CH:22]=[CH:21][CH:20]=[CH:19][C:10]=3[N:11]([CH2:12][CH:13]([CH3:18])[CH2:14][N:15]([CH3:17])[CH3:16])[C:4]=2[CH:3]=1

Participants

5

Reactant 3

HCID 24247Perchloric AcidHCID 129812TraboxopineHCID 444305L-Tartaric acid

Product 1

HCID 14555943HCID 14555943, compoundYield 87%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

To the filtrate obtained in Example 1, section A and having a volume of 110 to 120 cm3, 100 cm3 of dichloromethane are added and the base is deliberated as described in Example 1. To the dichloromethane solution containing 19.0 g of base as determined by means of titration with perchloric acid, an equivalent quantity of L(+)-tartaric acid is added under stirring. The mixture is stirred for several hours, the (+)-base L(+)-tartrate precipitated is filtered and dried. 21.6 g (87.0%) of (+)-2-chloro-12-(3-dimethylamino-2-methylpropyl)-12H-dibenzo[d,g][1,3,6]dioxazocine L(+)-tartrate are obtained, m.p.: 149°-152° C.

Workup

  1. additionare added
  2. stirringThe mixture is stirred for several hours
  3. customthe (+)-base L(+)-tartrate precipitated
  4. filtrationis filtered
  5. customdried

Sources & evidence

ORD record
ord-45c4951759dc4c4db0a9720a9758f4dc
Source dataset
uspto-grants-1990_03
Patent number
US04906622

Reaction notes

Loading…