Water → HCID 15729540, compound

HRID 704321Notes

Reaction equation

HRID 704321 reaction equation
[CH3:1][CH:2]([NH:4][S:5]([C:8]1[NH:9][C:10](=[O:14])[CH:11]=[CH:12][CH:13]=1)(=[O:7])=[O:6])[CH3:3].[CH3:15][S:16](Cl)(=[O:18])=[O:17].C(N(CC)CC)C.O>ClCCl>[CH3:3][CH:2]([NH:4][S:5]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][S:16]([CH3:15])(=[O:18])=[O:17])[N:9]=1)(=[O:7])=[O:6])[CH3:1]

Participants

6

Reactant 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 20074192HCID 20074192, compound

Product 1

HCID 15729540HCID 15729540, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent3×

Procedure

2-[(N-prop-2-yl)sulphamoyl]pyrid-6-one (0.052 g) was dissolved in dichloromethane (4 cm3). Methane sulphonylchloride (0.027 g) was added dropwise in dichloromethane (1 cm3) and the reaction mixture was stirred for 45 minutes. Triethylamine (0.024 g) in dichloromethane (1 cm3) was added dropwise and the reaction mixture was stirred for 2 hours. The mixture was left overnight and then refluxed for 2 hours. The cooled reaction mixture was poured into water and the product extracted into dichloromethane twice. The dichloromethane extracts were combined, dried, and evaporated under reduced pressure to leave the crude product.

Workup

  1. stirringthe reaction mixture was stirred for 2 hours
  2. waitThe mixture was left overnight
  3. temperaturerefluxed for 2 hours
  4. customThe cooled reaction mixture
  5. extractionthe product extracted into dichloromethane twice
  6. customdried
  7. customevaporated under reduced pressure

Sources & evidence

ORD record
ord-6d270193a17a420e88f1090aa5875270
Source dataset
uspto-grants-1991_01
Patent number
US04987141

Reaction notes

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