Phosphoric Acid → 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one

HRID 26500Notes

Reaction equation

HRID 26500 reaction equation
P(=O)(O)(O)[OH:2].CS([C:9]1[N:18]2[C:12]([CH2:13][C:14]3[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=3[CH:16]=[CH:17]2)=[N:11][N:10]=1)=O>O>[N:11]1[NH:10][C:9](=[O:2])[N:18]2[CH:17]=[CH:16][C:15]3[CH:19]=[CH:20][CH:21]=[CH:22][C:14]=3[CH2:13][C:12]=12

Participants

4

Reactant 2

HCID 1004Phosphoric AcidHCID 213235293-methylsulfinyl-11H-s-triazolo[3,4-b][3]benzazepine

Product 1

HCID 130667602,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To 3 ml of 80% phosphoric acid was added 0.245 g of 3-methylsulfinyl-11H-s-triazolo[3,4-b][3]benzazepine and the mixture was heated on an oil bath at 130°-140° C. for 1 hour. Following addition of water, the crystals were collected by filtration and dried. By the above procedure was obtained 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one. Recrystallization from chloroform-methanol yielded colorless needles, m.p. 210°-211° C.

Workup

  1. temperaturethe mixture was heated on an oil bath at 130°-140° C. for 1 hour
  2. filtrationthe crystals were collected by filtration
  3. customdried

Sources & evidence

ORD record
ord-b945d833e36e4dea9452fa24661f9e4c
Source dataset
uspto-grants-1979_04
Patent number
US04150139

Reaction notes

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