Water → HCID 19989021, compound

HRID 973722

Reaction equation

HRID 973722 reaction equation
[C:1](OC([O-])=O)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(C[NH:16][CH2:17][CH2:18][CH2:19][NH2:20])CN.O>C(Cl)Cl>[C:4]([O:3][C:1]([NH:20][CH:19]([CH2:19][CH2:18][CH2:17][NH2:16])[CH2:18][CH2:17][NH2:16])=[O:2])([CH3:7])([CH3:6])[CH3:5]

Participants

5

Reactant 3

HCID 962WaterHCID 5942Bis(3-aminopropyl)amineHCID 22064466Tert-butyldicarbonate

Product 1

HCID 19989021HCID 19989021, compoundYield 44.7%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

A solution of 33 g of tert-butyl dicarbonate in 200 ml of methylene chloride was added at 5° C. to a solution of 39.3 g of 3,3'-diaminodipropylamine in 300 ml of methylene chloride and after stirringf or 16 hours at 20° C., water was added, followed by decanting and evaporation to dryness. The residue was chromatographed on silica (eluant; methanol-ammonia (98-2)) to obtain 15.5 g of the expected product which was used as is for the next step.

Workup

  1. customby decanting
  2. customevaporation to dryness
  3. customThe residue was chromatographed on silica (eluant; methanol-ammonia (98-2))

Sources & evidence

ORD record
ord-9d3134bdfaae4dde982fa1a852abdee2
Source dataset
uspto-grants-1991_11
Patent number
US05064861

Linked notes

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