Sulfuric Acid → HCID 13338576, compound

HRID 2417915Notes

Reaction equation

HRID 2417915 reaction equation
S(=O)(=O)(O)O.[N+:6]([O-:9])(O)=[O:7].[N:10]1[CH2:11][CH2:12][CH2:13][N:14]2[C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=3[S:16][C:15]=12.[OH-].[NH4+]>>[N+:6]([C:21]1[CH:20]=[CH:19][C:18]2[N:14]3[CH2:13][CH2:12][CH2:11][N:10]=[C:15]3[S:16][C:17]=2[CH:22]=1)([O-:9])=[O:7]

Participants

4

Reactant 3

HCID 1118Sulfuric AcidHCID 14923Ammonium HydroxideHCID 20446979HCID 20446979, compound

Product 1

HCID 13338576HCID 13338576, compound

Procedure

To 92 parts of concentrated sulfuric acid are added portionwise 18.5 parts of 3,4-dihydro-2H-pyrimido[2,1-b]benzothiazole nitrate at 0° C. Upon completion, stirring is continued for 1 hour without cooling. The reaction mixture is poured onto 200 parts of ice-water and stirred for a while. The whole is alkalized with ammonium hydroxide and the product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The residue is stirred in 2,2'-oxybispropane. The product is filtered off and dried, yielding 16.3 parts of 3,4-dihydro-8-nitro-2H-pyrimido[2,1-b]benzothiazole; mp. 247.6° C.

Workup

  1. temperaturewithout cooling
  2. stirringstirred for a while
  3. extractionthe product is extracted with trichloromethane
  4. customThe extract is dried
  5. filtrationfiltered
  6. customevaporated
  7. stirringThe residue is stirred in 2,2'-oxybispropane
  8. filtrationThe product is filtered off
  9. customdried

Sources & evidence

ORD record
ord-db3078afa7434b40918d3392bf460eda
Source dataset
uspto-grants-1984_09
Patent number
US04471117

Reaction notes

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