4-Iodophenol → HCID 10120988, compound

HRID 1835589Notes

Reaction equation

HRID 1835589 reaction equation
I[C:2]1C=CC(O)=CC=1.C(=O)([O-])[O-].[K+].[K+].[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]2[CH:54]=[CH:53][C:52]([O:55][CH3:56])=[CH:51][C:23]=2[CH2:24][O:25][C:26]2[CH:31]=[CH:30][C:29]([C:32]3[N:36]([CH:37]4[CH2:42][CH2:41][CH2:40][CH2:39][CH2:38]4)[C:35]4[CH:43]=[CH:44][C:45]([C:47]([O:49][CH3:50])=[O:48])=[CH:46][C:34]=4N=3)=[CH:28][CH:27]=2)=[CH:18][CH:17]=1>CC(C)=O>[Cl:15][C:16]1[CH:17]=[CH:18][C:19]([C:22]2[CH:54]=[CH:53][C:52]([O:55][CH3:56])=[CH:51][C:23]=2[CH2:24][O:25][C:26]2[CH:27]=[CH:28][C:29]([C:32]3[N:36]([CH:37]4[CH2:38][CH2:39][CH2:40][CH2:41][CH2:42]4)[C:35]4[C:34]([CH:2]=3)=[CH:46][C:45]([C:47]([O:49][CH3:50])=[O:48])=[CH:44][CH:43]=4)=[CH:30][CH:31]=2)=[CH:20][CH:21]=1

Participants

5

Procedure

4-Iodophenol (5.0 g) was dissolved in acetone (50 ml), and potassium carbonate (4.7 g) and 4′-chloro-2-chloromethyl-4-methoxybiphenyl (6.0 g) obtained in Example 241, Step 4 were added. The mixture was refluxed for 10 hr. The reaction mixture was concentrated and 4N aqueous sodium hydroxide solution (50 ml) was added. The precipitated crystals were collected by filtration, washed with water, and dried under reduced pressure to give the title compound (10.0 g, yield 98%).

Workup

  1. temperatureThe mixture was refluxed for 10 hr
  2. concentrationThe reaction mixture was concentrated
  3. addition4N aqueous sodium hydroxide solution (50 ml) was added
  4. filtrationThe precipitated crystals were collected by filtration
  5. washwashed with water
  6. customdried under reduced pressure

Sources & evidence

ORD record
ord-fb458979c6604897aff601d297723a0f
Source dataset
uspto-grants-2004_08
Patent number
US06770666B2

Reaction notes

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