Ammonia → HCID 13120754, compound

HRID 1462639Notes

Reaction equation

HRID 1462639 reaction equation
C([O:3][C:4](=O)[CH2:5][N:6]1[C:10]2[CH2:11][N:12]=[C:13]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:14]3[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][C:15]=3[C:9]=2[CH:8]=[N:7]1)C.[NH3:28]>>[Cl:20][C:18]1[CH:17]=[CH:16][C:15]2[C:9]3[CH:8]=[N:7][N:6]([CH2:5][C:4]([NH2:28])=[O:3])[C:10]=3[CH2:11][N:12]=[C:13]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[C:14]=2[CH:19]=1

Participants

3

Reactant 2

HCID 222AmmoniaHCID 53903404HCID 53903404, compound

Product 1

HCID 13120754HCID 13120754, compound

Procedure

A mixture of 0.4 g (1.05 mmol) of 8-chloro-6-phenyl-3H,4H-pyrazolo[3,4-d][2]benzazepine-3-acetic acid ethyl ester and 20 ml of methanolic ammonia (ca 20% v/v) was heated in an autoclave on the steam bath overnight. The solvent was evaporated and the residue was purified by chromatography over 15 g of silica gel using 5% (v/v) of ethanol in methylene chloride. Crystallization from ethyl acetate/ether gave colorless crystals with mp 218°-219°.

Workup

  1. temperaturewas heated in an autoclave on the steam bath overnight
  2. customThe solvent was evaporated
  3. customthe residue was purified by chromatography over 15 g of silica gel using 5% (v/v) of ethanol in methylene chloride
  4. customCrystallization from ethyl acetate/ether
  5. customgave colorless crystals with mp 218°-219°

Sources & evidence

ORD record
ord-1e848fe4fcc74cd89ee8788b500a74b0
Source dataset
uspto-grants-1984_07
Patent number
US04460781

Reaction notes

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