Ethanol → HCID 10950582, compound

HRID 1384499Notes

Reaction equation

HRID 1384499 reaction equation
NN.C(O)C.[C:6]([O:10][C:11]([N:13]([CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][N:47]1C(=O)C2=CC=CC=C2C1=O)[CH2:14][CH2:15][N:16]([C:34]([O:36][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:35])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][N:23]1C(=O)C2=CC=CC=C2C1=O)=[O:12])([CH3:9])([CH3:8])[CH3:7]>C(Cl)Cl>[NH2:47][CH2:46][CH2:45][CH2:44][CH2:43][CH2:42][CH2:41][N:13]([C:11]([O:10][C:6]([CH3:9])([CH3:8])[CH3:7])=[O:12])[CH2:14][CH2:15][N:16]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][NH2:23])[C:34]([O:36][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:35]

Participants

5

Reactant 3

HCID 702EthanolHCID 9321HydrazineHCID 11125419HCID 11125419, compound

Product 1

HCID 10950582HCID 10950582, compoundYield 84%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A solution of anhydrous hydrazine (1 ml) was added to a stirred mixture of anhydrous ethanol (30 ml) and methylene chloride (20 ml) containing N,N′-bis(t-butyloxycarbonyl)-N,N′-bis(6-phthalimidohexyl)-1,2-diaminoethane (2.8 g; example 9). The reaction was continued overnight and the precipitated phthalazinedione by-product was removed by filtration. The filtrate on concentration at reduced pressure gave the title compound (1.5 g) as an oil.

Workup

  1. customthe precipitated phthalazinedione by-product was removed by filtration
  2. concentrationThe filtrate on concentration at reduced pressure

Sources & evidence

ORD record
ord-fc5451e8f56749dd8efc303e57477b95
Source dataset
uspto-grants-2001_07
Patent number
US06258976B1

Reaction notes

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