Benzylamine → HCID 21922997, compound

HRID 1272623Notes

Reaction equation

HRID 1272623 reaction equation
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH:11]([CH3:14])[CH2:12][CH3:13])=[C:4](Cl)[N:3]=1.[CH2:16]([NH2:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C(O)CCC>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH:11]([CH3:14])[CH2:12][CH3:13])=[C:4]([NH:23][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:3]=1

Participants

4

Reactant 2

HCID 7504BenzylamineHCID 21922929HCID 21922929, compound

Product 1

HCID 21922997HCID 21922997, compound

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Conditions

Temperature
100 °C

Procedure

The operation is carried out as in Stage 2 of Example 3 and 161 mg of the product obtained in Stage 1 above, 3 ml of butanol and 0,132 ml of benzylamine are mixed together and the reaction medium is heated to a temperature of approximately 90 to 110° C. for approximately 5 hours, then left to return to ambient temperature. After leaving to crystallize, the reaction medium is diluted with 10 ml of isopropanol, followed by separating, washing with 10 ml of isopropanol and drying under vacuum at approximately 50° C. After chromatography on silica eluting with methylene chloride/ethyl acetate in a proportion of 50/50, In this way 179 mg of expected product is obtained in the form of white crystals.

Workup

  1. additionare mixed together
  2. waitleft
  3. customto return to ambient temperature
  4. customAfter leaving
  5. customto crystallize
  6. additionthe reaction medium is diluted with 10 ml of isopropanol
  7. customby separating
  8. washwashing with 10 ml of isopropanol
  9. customdrying under vacuum at approximately 50° C

Sources & evidence

ORD record
ord-7fd77467412b4ed7abdaa57e08418a5d
Source dataset
uspto-grants-2007_04
Patent number
US07208598B2

Reaction notes

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