Hydrochloric Acid → HCID 68520012, compound

HRID 748897Notes

Reaction equation

HRID 748897 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([C:12]2[C:13]([O:23][C:24]3[CH:29]=[CH:28][C:27]([O:30][CH2:31][CH2:32][N:33]4[CH2:38][CH2:37][CH2:36][CH2:35][CH2:34]4)=[CH:26][CH:25]=3)=[C:14]3[C:19](=[CH:20][CH:21]=2)[CH:18]=[C:17]([OH:22])[CH:16]=[CH:15]3)[CH:5]=[CH:6][C:7]=1[S:8]([CH3:11])(=[O:10])=[O:9].Cl>C(OCC)C.C(OCC)(=O)C.CO>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([C:12]2[C:13]([O:23][C:24]3[CH:29]=[CH:28][C:27]([O:30][CH2:31][CH2:32][N:33]4[CH2:34][CH2:35][CH2:36][CH2:37][CH2:38]4)=[CH:26][CH:25]=3)=[C:14]3[C:19](=[CH:20][CH:21]=2)[CH:18]=[C:17]([OH:22])[CH:16]=[CH:15]3)[CH:5]=[CH:6][C:7]=1[S:8]([CH3:11])(=[O:10])=[O:9]

Participants

6

Reactant 2

HCID 313Hydrochloric AcidHCID 68517827HCID 68517827, compound

Product 1

HCID 68520012HCID 68520012, compoundYield 26%

Reagents, catalysts & solvents 3

HCID 887MethanolSolventHCID 3283Diethyl EtherSolvent2×HCID 8857Ethyl AcetateSolvent

Procedure

Dissolve the product of Example 29 in diethyl ether (5.0 mL), ethyl acetate (6.0 mL) and methanol (1.0 mL) and add 2M HCl in diethyl ether (0.6 mL, 1.2 mmol). Collect the precipitate on filter paper, rinse with diethyl ether and dry in vacuo (<2 mm of Hg) at 20° C. for 4 hours to give 16 mg of the title compound (26%): mass spectrum (ion spray): m/z=552.3 (M+H—HCl).

Workup

  1. customCollect the precipitate
  2. filtrationon filter paper
  3. washrinse with diethyl ether
  4. customdry in vacuo (<2 mm of Hg) at 20° C. for 4 hours

Sources & evidence

ORD record
ord-81e9ff56fa5f496685fbd5c19ba4bf61
Source dataset
uspto-grants-2008_07
Patent number
US07399867B2

Reaction notes

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