HCID 46224497, compound → HCID 11512800, compound

HRID 1994182Notes

Reaction equation

HRID 1994182 reaction equation
O.[C:2]1([S:16]([OH:19])(=[O:18])=[O:17])[C:11]2[CH:10]=[CH:9][CH:8]=[C:7]([S:12]([OH:15])(=[O:14])=[O:13])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[Cl:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[C@H:27]([N:32]1[CH2:37][CH2:36][C:35]2[S:38][CH:39]=[CH:40][C:34]=2[CH2:33]1)[C:28]([O:30][CH3:31])=[O:29]>C(#N)C>[C:2]1([S:16]([OH:19])(=[O:18])=[O:17])[C:11]2[CH:10]=[CH:9][CH:8]=[C:7]([S:12]([OH:15])(=[O:14])=[O:13])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[Cl:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[C@H:27]([N:32]1[CH2:37][CH2:36][C:35]2[S:38][CH:39]=[CH:40][C:34]=2[CH2:33]1)[C:28]([O:30][CH3:31])=[O:29]

Participants

3

Reactant 1

HCID 46224497HCID 46224497, compound

Product 1

HCID 11512800HCID 11512800, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

Form B of methyl(+)-(S)-α-(2-chlorophenyl)-6,7-dihydrothieno[3,2-C]pyridine-5(4H) acetate naphthalene-1,5-disulfonate hydrate of Example 2 (0.0616 g) was dissolved in acetonitrile (1.0 mL) with sonication. The solution was filtered through a 0.2 μm nylon filter into a clean vial which was placed in a larger vial containing isopropylacetate (2.0 mL). The larger vial was capped and crystallization was afforded by vapor diffusion to afford the title compound in the form of an amorphous solid which was analyzed by FTIR and XRPD.

Workup

  1. filtrationThe solution was filtered through a 0.2 μm nylon
  2. filtrationfilter into a clean vial which
  3. additioncontaining isopropylacetate (2.0 mL)
  4. customThe larger vial was capped
  5. customcrystallization
  6. customwas afforded by vapor diffusion

Sources & evidence

ORD record
ord-e7e09fd557c9425085a8fe98bbfbade2
Source dataset
uspto-grants-2010_01
Patent number
US07652139B2

Reaction notes

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