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

HRID 1450381Notes

Reaction equation

HRID 1450381 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 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 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-e580811aeec2475e816128dc5bce837d
Source dataset
uspto-grants-1997_02
Patent number
US05602137

Reaction notes

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