Hydrochloric Acid → HCID 59304992, compound

HRID 2240269Notes

Reaction equation

HRID 2240269 reaction equation
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]2[NH:16][CH:17]=[CH:18][C:11]=12.[Cl:19][C:20]1[CH:25]=[C:24](Cl)[N:23]=[C:22]([NH2:27])[N:21]=1.Cl.[OH-].[Na+]>O>[Cl:19][C:20]1[N:21]=[C:22]([NH2:27])[N:23]=[C:24]([NH:8][C:6]2[CH:5]=[CH:4][C:3]([NH:9][C:10]3[CH:15]=[CH:14][N:13]=[C:12]4[NH:16][CH:17]=[CH:18][C:11]=34)=[C:2]([Cl:1])[CH:7]=2)[CH:25]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 655222-Amino-4,6-dichloropyrimidineHCID 59305028HCID 59305028, compound

Product 1

HCID 59304992HCID 59304992, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
100 °C

Procedure

27 mg (0.10 mmol) of 2-chloro-N1-1H-pyrrolo[2,3-b]pyridin-4-ylbenzene-1,4-diamine and 24 mg (0.15 mmol) of 4,6-dichloropyrimidine-2-amine are suspended in 5 ml of water. 0.14 ml of 1 M hydrochloric acid are added, and the mixture is heated at 100° C. overnight. Using 1N aqueous sodium hydroxide solution, the suspension is then adjusted to pH 10, resulting in the precipitation of crystals. The solid is filtered off and washed with water. The crude product is purified by preparative HPLC.

Workup

  1. customresulting in the precipitation of crystals
  2. filtrationThe solid is filtered off
  3. washwashed with water
  4. customThe crude product is purified by preparative HPLC

Sources & evidence

ORD record
ord-8a697e6148364ec6a9fa30abda376f2e
Source dataset
uspto-grants-2010_05
Patent number
US07723347B2

Reaction notes

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