Acetic Anhydride → HCID 13338631, compound

HRID 2417922Notes

Reaction equation

HRID 2417922 reaction equation
C(O[C:5](=[O:7])[CH3:6])(=O)C.[N:8]1[CH2:9][CH2:10][CH2:11][N:12]2[C:16]3[CH:17]=[C:18]([NH2:21])[CH:19]=[CH:20][C:15]=3[S:14][C:13]=12>>[N:8]1[CH2:9][CH2:10][CH2:11][N:12]2[C:16]3[CH:17]=[C:18]([NH:21][C:5](=[O:7])[CH3:6])[CH:19]=[CH:20][C:15]=3[S:14][C:13]=12

Participants

3

Reactant 2

HCID 7918Acetic AnhydrideHCID 133385843,4-Dihydro-2H-pyrimido[2,1-b][1,3]benzothiazol-7-amine

Product 1

HCID 13338631HCID 13338631, compound

Procedure

To 25 parts of acetic acid anhydride are added portionwise 1.3 parts of 3,4-dihydro-2H-pyrimido[2,1-b]benzothiazol-7-amine (exothermic reaction: temp. rises to 30° C.). Upon completion, stirring is continued for one hour at room temperature. After cooling to 5°-10° C., the precipitated product is filtered off and dissolved in water. The solution is treated with activated charcoal. The latter is filtered off over hyflo and the filtrate is alkalized with a few drops of ammonium hydroxide. Upon stirring, the product is allowed to crystallize. It is filtered off and dried, yielding 0.8 parts of N-(3,4-dihydro-2H-pyrimido[2,1-b]benzothiazol-7-yl)acetamide; mp. 178° C.

Workup

  1. temperatureAfter cooling to 5°-10° C.
  2. filtrationthe precipitated product is filtered off
  3. dissolutiondissolved in water
  4. additionThe solution is treated with activated charcoal
  5. filtrationThe latter is filtered off over hyflo
  6. stirringUpon stirring
  7. customto crystallize
  8. filtrationIt is filtered off
  9. customdried

Sources & evidence

ORD record
ord-6c79ee46d34c4fef968c8a99cf03eb6d
Source dataset
uspto-grants-1984_09
Patent number
US04471117

Reaction notes

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