3H-2,1-Benzoxathiol-3-one 1,1-dioxide → HCID 19975838, compound

HRID 1898899Notes

Reaction equation

HRID 1898899 reaction equation
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[N:14]3[N:15]=[CH:16][CH:17]=[C:13]3[N:12]=[C:11]([CH2:18][CH3:19])[CH:10]=2)=[CH:4][CH:3]=1.[CH:20]1[CH:25]=[C:24]2[C:26]([O:28][S:29](=[O:31])(=[O:30])[C:23]2=[CH:22][CH:21]=1)=[O:27]>ClCCl>[CH2:18]([C:11]1[CH:10]=[C:9]([NH:8][C:5]2[CH:4]=[CH:3][C:2]([NH:1][C:26]([C:24]3[CH:25]=[CH:20][CH:21]=[CH:22][C:23]=3[S:29]([OH:31])(=[O:30])=[O:28])=[O:27])=[CH:7][CH:6]=2)[N:14]2[N:15]=[CH:16][CH:17]=[C:13]2[N:12]=1)[CH3:19]

Participants

4

Reactant 2

HCID 657293H-2,1-Benzoxathiol-3-one 1,1-dioxideHCID 19975979HCID 19975979, compound

Product 1

HCID 19975838HCID 19975838, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

1.3 g (5.1 mmol) of the amine from Example 14, Step B and 940 mg (5.1 mmol) of 2-sulfobenzoic acid cyclic anhydride were dissolved in 20 ml dichloromethane. A solid material precipitated immediately from the clear solution, and the mixture was stirred at room temperature over night. The the pale yellow crystals of the title compound were filtered by suction, heated with ethanol, filtered again after cooling to room temperature, and dried in vacuo, m.p.>320° C.

Workup

  1. customA solid material precipitated immediately from the clear solution
  2. filtrationThe the pale yellow crystals of the title compound were filtered by suction
  3. temperatureheated with ethanol
  4. filtrationfiltered again
  5. temperatureafter cooling to room temperature
  6. customdried in vacuo, m.p.>320° C.

Sources & evidence

ORD record
ord-534c4cb2199a4736a91f563cedd6c7f2
Source dataset
uspto-grants-1996_11
Patent number
US05571813

Reaction notes

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