Bromine → HCID 68119070, compound

HRID 1580563Notes

Reaction equation

HRID 1580563 reaction equation
[Br:1]Br.[N+:3]([CH:6]=[C:7]1[NH:12][CH2:11][CH2:10][CH2:9][S:8]1)([O-:5])=[O:4]>C(Cl)Cl.O>[Br:1][C:6]([N+:3]([O-:5])=[O:4])=[C:7]1[NH:12][CH2:11][CH2:10][CH2:9][S:8]1

Participants

5

Reactant 2

HCID 24408BromineHCID 428532-nitromethylenetetrahydro-2H-1,3-thiazine

Product 1

HCID 68119070HCID 68119070, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6344DichloromethaneSolvent2×

Procedure

A solution of 3.2 g of bromine in 10 ml of methylene chloride was added dropwise to a solution of 3.2 g of 1A in 50 ml of water, the temperature being held at 5°-10°. The mixture was then stirred for 45 minutes when 200 ml of methylene chloride was added to dissolve the solid material. The organic phase was separated, washed with water, dried (Na2SO4) and concentrated under reduced pressure to give a yellow solid. This was washed with ether to give 2A as a yellow solid, m.p. 122° (with decomposition).

Workup

  1. custombeing held at 5°-10°
  2. additionwas added
  3. dissolutionto dissolve the solid material
  4. customThe organic phase was separated
  5. washwashed with water
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated under reduced pressure
  8. customto give a yellow solid
  9. washThis was washed with ether

Sources & evidence

ORD record
ord-a5b2e4f0b54d4046b8d83d3cd3024035
Source dataset
uspto-grants-1976_01
Patent number
US03933809

Reaction notes

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