Hydrochloric Acid → HCID 10487762, compound

HRID 2210440Notes

Reaction equation

HRID 2210440 reaction equation
[S:1]1(=[O:12])(=[O:11])[C:6]2[CH:7]=[CH:8][CH:9]=[N:10][C:5]=2[NH:4][CH:3]=[N:2]1.[BH4-].[Na+].Cl>O>[S:1]1(=[O:11])(=[O:12])[C:6]2[CH:7]=[CH:8][CH:9]=[N:10][C:5]=2[NH:4][CH2:3][NH:2]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 30540122H-Pyrido(2,3-e)-1,2,4-thiadiazine, 1,1-dioxideHCID 4311764Sodium borohydride

Product 1

HCID 10487762HCID 10487762, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

1 g of 4H-pyrido[2,3-e][1,2,4]thiadiazine 1,1- dioxide is suspended in 30 cm3 of water. A solution of 0.83 g of NaBH4 in 5 cm3 of water is added to the suspension. After stirring for 15 minutes at ambient temperature, the pH of the solution is adjusted to 6.5-7 using dilute HCl. The precipitate obtained is filtered, washed with water and dried. The dried compound is dissolved in 200 cm3 of dichloromethane. The possible insoluble material is removed by filtration. The filtrate is treated with an equal volume of petroleum ether (40°-60° C.) and placed at +4° C. overnight. The crystals obtained are collected on a filter and dried.

Workup

  1. customThe precipitate obtained
  2. filtrationis filtered
  3. washwashed with water
  4. customdried
  5. dissolutionThe dried compound is dissolved in 200 cm3 of dichloromethane
  6. customThe possible insoluble material is removed by filtration
  7. additionThe filtrate is treated with an equal volume of petroleum ether (40°-60° C.)
  8. waitplaced at +4° C. overnight
  9. customThe crystals obtained
  10. customare collected on
  11. filtrationa filter
  12. customdried

Sources & evidence

ORD record
ord-f42d5bf4ac4a429ea70bd9c6d78c5b8a
Source dataset
uspto-grants-1995_10
Patent number
US05459138

Reaction notes

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