HCID 21923033, compound → HCID 178478740, compound

HRID 1272671Notes

Reaction equation

HRID 1272671 reaction equation
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH:11]2[CH2:15][CH2:14][CH2:13][CH2:12]2)=[C:4]([NH:16][CH2:17][CH2:18][NH:19][C:20](=[O:29])[C:21]2[CH:26]=[C:25]([Cl:27])[CH:24]=[C:23]([Cl:28])[CH:22]=2)[N:3]=1.[NH2:30][C@H:31]1[CH2:36][CH2:35][C@H:34]([NH2:37])[CH2:33][CH2:32]1>>[ClH:1].[ClH:1].[NH2:30][C@H:31]1[CH2:36][CH2:35][C@H:34]([NH:37][C:2]2[N:10]=[C:9]3[C:5]([N:6]=[CH:7][N:8]3[CH:11]3[CH2:15][CH2:14][CH2:13][CH2:12]3)=[C:4]([NH:16][CH2:17][CH2:18][NH:19][C:20](=[O:29])[C:21]3[CH:22]=[C:23]([Cl:28])[CH:24]=[C:25]([Cl:27])[CH:26]=3)[N:3]=2)[CH2:33][CH2:32]1

Participants

3

Reactant 2

HCID 21923033HCID 21923033, compoundHCID 178511674HCID 178511674, compound

Product 1

HCID 178478740HCID 178478740, compound

Conditions

Temperature
140 °C

Procedure

360 mg of the product obtained in Stage 1 above and 450 mg of trans-1,4-diaminocyclohexane are mixed together and the reaction medium is heated to approximately 140° C. for 6 hours. After evaporating the solvent, chromatography on silica is carried out (eluent methylene chloride/ methanol/ammonium hydroxide 85/15/1.5) followed by taking up in an ethanolic solution of hydrochloric acid, leaving to crystallize, separating, drying under reduced pressure and 280 mg of expected product is recovered.

Workup

  1. customAfter evaporating the solvent, chromatography on silica
  2. customleaving
  3. customto crystallize
  4. customseparating
  5. dry with materialdrying under reduced pressure and 280 mg of expected product
  6. customis recovered

Sources & evidence

ORD record
ord-9b89143ad9e64ee5ae65d6ee2dc79676
Source dataset
uspto-grants-2007_04
Patent number
US07208598B2

Reaction notes

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