Iodine → HCID 57636978, compound

HRID 2110927Notes

Reaction equation

HRID 2110927 reaction equation
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.II.C(N(CC)CC)C.[C:29]([O:33][C:34](=[O:46])[NH:35][CH2:36][CH2:37][C:38](=[O:45])[NH:39][NH:40][C:41](=O)[CH2:42][CH3:43])([CH3:32])([CH3:31])[CH3:30]>ClCCl>[C:29]([O:33][C:34](=[O:46])[NH:35][CH2:36][CH2:37][C:38]1[O:45][C:41]([CH2:42][CH3:43])=[N:40][N:39]=1)([CH3:32])([CH3:31])[CH3:30]

Participants

6

Reactant 4

HCID 807IodineHCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 57637130HCID 57637130, compound

Product 1

HCID 57636978HCID 57636978, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

11.49 g (24.70 mmol) PS-triphenylphosphine are placed in 240 ml dichloromethane, 6.27 g (24.70 mmol) iodine are added. The mixture is stirred for 0.1 hours at ambient temperature, then 7.00 ml (50.50 mmol) triethylamine are added dropwise. 3.20 g (12.34 mmol) tert-butyl[3-oxo-3-(N′-propionyl-hydrazino)-propyl]-carbamate dissolved in 150 ml dichloromethane are added. The reaction mixture is stirred for 24 hours at ambient temperature, then the precipitate is filtered off. The filtrate is evaporated down and purified by chromatography.

Workup

  1. additionare added
  2. stirringThe reaction mixture is stirred for 24 hours at ambient temperature
  3. filtrationthe precipitate is filtered off
  4. customThe filtrate is evaporated down
  5. custompurified by chromatography

Sources & evidence

ORD record
ord-f2f72ade585d4984b6f73ea576134e9a
Source dataset
uspto-grants-2009_04
Patent number
US07517995B2

Reaction notes

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