Potassium Carbonate → HCID 60045681, compound

HRID 1064590Notes

Reaction equation

HRID 1064590 reaction equation
[NH2:1][C:2]1[CH:3]=[C:4]([S:8]([N:11]2[C@@H:16]([CH3:17])[CH2:15][N:14]([CH2:18][C:19]([NH:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[CH3:28])=[O:20])[CH2:13][C@H:12]2[CH3:29])(=[O:10])=[O:9])[CH:5]=[CH:6][CH:7]=1.[CH3:30][S:31](Cl)(=[O:33])=[O:32].C([O-])([O-])=O.[K+].[K+]>C(O)C.O>[CH3:30][S:31]([NH:1][C:2]1[CH:3]=[C:4]([S:8]([N:11]2[C@@H:16]([CH3:17])[CH2:15][N:14]([CH2:18][C:19]([NH:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[CH3:28])=[O:20])[CH2:13][C@H:12]2[CH3:29])(=[O:9])=[O:10])[CH:5]=[CH:6][CH:7]=1)(=[O:33])=[O:32]

Participants

6

Reactant 3

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 60045700HCID 60045700, compound

Product 1

HCID 60045681HCID 60045681, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

The title compound was prepared from the product of Example 57 and methane sulphonyl chloride by the method of Example 62. The solid obtained at the end of the reaction was suspended in ethanol (50 ml) to which a solution of K2CO3 (0.2 g) in water (10 ml) was added, and stirred for 18 hours, in order to hydrolyse any bis-sulphonamide. The ethanol was removed, water (50 ml) was added and the pH was adjusted to 5.0. The solid was filtered off, washed with water and ether and dried in vacuo to give the title compound as a white solid. Yield 0.13 g.

Workup

  1. customThe solid obtained at the end of the reaction
  2. additionwas added
  3. customThe ethanol was removed
  4. additionwater (50 ml) was added
  5. filtrationThe solid was filtered off
  6. washwashed with water and ether
  7. customdried in vacuo

Sources & evidence

ORD record
ord-8b84bc0be04d4f7ab1a01373bcb53431
Source dataset
uspto-grants-2005_11
Patent number
US06969713B2

Reaction notes

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