Ammonium Hydroxide → HCID 59198483, compound

HRID 1896551Notes

Reaction equation

HRID 1896551 reaction equation
Cl[C:2]1[C:14]2[C:13]3[CH:12]=[CH:11][C:10]([C:15]([F:18])([F:17])[F:16])=[CH:9][C:8]=3[N:7]([CH3:19])[C:6]=2[C:5]([C:20]#[N:21])=[CH:4][N:3]=1.[NH4+:22].[OH-]>CCO>[NH2:22][C:2]1[C:14]2[C:13]3[CH:12]=[CH:11][C:10]([C:15]([F:18])([F:17])[F:16])=[CH:9][C:8]=3[N:7]([CH3:19])[C:6]=2[C:5]([C:20]#[N:21])=[CH:4][N:3]=1

Participants

4

Reactant 2

HCID 14923Ammonium HydroxideHCID 86639256HCID 86639256, compound

Product 1

HCID 59198483HCID 59198483, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
145 °C

Procedure

The product of Step 2 was dissolved in a 2:3 (v/v) mixture of EtOH and conc. NH4OH (0.027 M) in a stainless steel Parr pressure vessel. The vessel was sealed and the reaction was heated for 16 h at 145° C. After cooling to 0° C., the mixture was concentrated to dryness under vacuum and the resulting solid was stirred with 1:10 EtOAc:hexanes containing 10% MeOH to give the title compound as an off-white solid.

Workup

  1. customThe vessel was sealed
  2. temperatureAfter cooling to 0° C.
  3. concentrationthe mixture was concentrated to dryness under vacuum

Sources & evidence

ORD record
ord-d8aae8ce5fbf4bf78cc1e75938d27924
Source dataset
uspto-grants-2013_08
Patent number
US08518964B2

Reaction notes

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