Azane;hydrate → HCID 135990571, compound

HRID 2257511Notes

Reaction equation

HRID 2257511 reaction equation
[I:1][C:2]1[CH:16]=[CH:15][C:5]2[N:6]=[C:7]([C:11]([F:14])([F:13])[F:12])[O:8][C:9](=O)[C:4]=2[CH:3]=1.O.[NH3:18]>>[I:1][C:2]1[CH:3]=[C:4]2[C:5](=[CH:15][CH:16]=1)[N:6]=[C:7]([C:11]([F:14])([F:13])[F:12])[NH:18][C:9]2=[O:8]

Participants

3

Reactant 2

HCID 12896473Azane;hydrateHCID 17349916HCID 17349916, compound

Product 1

HCID 135990571HCID 135990571, compound

Conditions

Temperature
0 °C

Procedure

6-iodo-2-trifluoromethyl-benzo[d][1,3] oxazin-4-one (0.6 g, 1.76 mmole) was stirred with 25 mL of concentrated ammonia water at 40° C. for 5 h, cooled to 0° C., the precipitate was filtered and dried under vacuo. The product was recrystallized from ethyl acetate and haxanes to give 0.58 g, mp >255° C. (sub), MS (CI): m/z 341 (MH)+.

Workup

  1. filtrationthe precipitate was filtered
  2. customdried under vacuo
  3. customThe product was recrystallized from ethyl acetate and haxanes
  4. customto give 0.58 g, mp >255° C. (sub), MS (CI)

Sources & evidence

ORD record
ord-08386ec5582b4fb78c9aa322de66ebdc
Source dataset
uspto-grants-1997_08
Patent number
US05658902

Reaction notes

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