1-Butanol → HCID 21923017, compound

HRID 1244929Notes

Reaction equation

HRID 1244929 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.C(O)CCC.[CH2:21]([NH2:24])[CH2:22][CH3:23]>C(OCC)(=O)C>[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:24][CH2:21][CH2:22][CH3:23])[N:3]=1

Participants

5

Reactant 3

HCID 2631-ButanolHCID 7852PropylamineHCID 21922929HCID 21922929, compound

Product 1

HCID 21923017HCID 21923017, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

The operation is carried out as in Stage 2 of Example 9 starting from 200 mg of the product obtained in Stage 1 of Example 9 and 4 ml of butanol and using 0.132 ml 1-propanamine in place of the benzylamine. Agitation is carried out at ambient temperature then the reaction medium is taken to a temperature of 80 to 85° C. for approximately 22 hours, left to return to ambient temperature, followed by taking up in 5 ml of ethyl acetate, evaporating to dryness, impasting in 5 ml of pentane at ambient temperature, separating, washing with 5 ml of pentane and drying at a temperature of approximately 50° C.

Workup

  1. customis carried out at ambient temperature
  2. waitleft
  3. customto return to ambient temperature
  4. customevaporating to dryness
  5. customimpasting in 5 ml of pentane at ambient temperature
  6. customseparating
  7. washwashing with 5 ml of pentane
  8. customdrying at a temperature of approximately 50° C.

Sources & evidence

ORD record
ord-5b9512c9d3b946559174441a34f02851
Source dataset
uspto-grants-2006_10
Patent number
US07122669B1

Reaction notes

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