Sodium Carbonate → HCID 178441669, compound

HRID 1377516Notes

Reaction equation

HRID 1377516 reaction equation
[CH2:1]([C:5]1[N:9]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]3[N:27](C(OCC)C)[N:26]=[N:25][N:24]=3)=[CH:13][CH:12]=2)[C:8]([CH:33]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([CH:41]([O:44][CH3:45])[O:42][CH3:43])[N:36]=2)[OH:34])=[C:7]([Cl:46])[N:6]=1)[CH2:2][CH2:3][CH3:4].Cl.CO.C([O-])([O-])=O.[Na+].[Na+]>>[CH2:1]([C:5]1[N:9]([CH2:10][C:11]2[CH:12]=[CH:13][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]3[NH:27][N:26]=[N:25][N:24]=3)=[CH:15][CH:16]=2)[C:8]([CH:33]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([CH:41]([O:42][CH3:43])[O:44][CH3:45])[N:36]=2)[OH:34])=[C:7]([Cl:46])[N:6]=1)[CH2:2][CH2:3][CH3:4]

Participants

4

Reactant 3

HCID 10340Sodium CarbonateHCID 21893726Hydrochloride methanolHCID 22914865HCID 22914865, compound

Product 1

HCID 178441669HCID 178441669, compoundYield 85.3%

Procedure

To 50 mg (0.077 mmole) of the compound obtained in step 1 of Example 1 was added 1 ml of 3% hydrogen chloride/methanol solution and the resulting solution was stirred for 10 minutes at room temperature. After being added with a small amount of Na2CO3, the resultant was concentrated under reduced pressure and purified with silica gel column chromatography to obtain 37.7 mg of the title compound (yield 85%).

Workup

  1. concentrationthe resultant was concentrated under reduced pressure
  2. custompurified with silica gel column chromatography

Sources & evidence

ORD record
ord-45355be31e4c42b88ef8bc681c33affc
Source dataset
uspto-grants-1997_09
Patent number
US05665738

Reaction notes

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