Sodium Hydroxide → 2-Hydroxy-4-[7-(1-adamantyl)-6-benzyloxy-2-naphthyl]benzoic acid

HRID 618482Notes

Reaction equation

HRID 618482 reaction equation
[OH:1][C:2]1[CH:11]=[C:10]([C:12]2[CH:21]=[CH:20][C:19]3[C:14](=[CH:15][C:16]([C:30]45[CH2:39][CH:34]6[CH2:35][CH:36]([CH2:38][CH:32]([CH2:33]6)[CH2:31]4)[CH2:37]5)=[C:17]([O:22][CH2:23][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)[CH:18]=3)[CH:13]=2)[CH:9]=[CH:8][C:3]=1[C:4]([O:6]C)=[O:5].[OH-].[Na+]>>[OH:1][C:2]1[CH:11]=[C:10]([C:12]2[CH:21]=[CH:20][C:19]3[C:14](=[CH:15][C:16]([C:30]45[CH2:37][CH:36]6[CH2:38][CH:32]([CH2:33][CH:34]([CH2:35]6)[CH2:39]4)[CH2:31]5)=[C:17]([O:22][CH2:23][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)[CH:18]=3)[CH:13]=2)[CH:9]=[CH:8][C:3]=1[C:4]([OH:6])=[O:5]

Participants

3

Procedure

930 mg (1.8 mmol) of methyl 2-hydroxy-4-[7-(1-adamantyl)-6-benzyloxy-2-naphthyl]benzoate and 100 ml of a 2N methanolic sodium hydroxide solution were introduced into a round-bottomed flask and the reaction mixture was heated at reflux for one hour. The reaction mixture was evaporated to dryness, the residue was taken up in water and acidified to pH 1 with concentrated hydrochloric acid and the solid was filtered. The solid obtained was triturated in ethyl acetate, filtered and dried. 710 mg (79%) of the expected acid were collected, which acid had a melting point of 263°-4° C.

Workup

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux for one hour
  3. customThe reaction mixture was evaporated to dryness
  4. filtrationthe solid was filtered
  5. customThe solid obtained
  6. customwas triturated in ethyl acetate
  7. filtrationfiltered
  8. customdried
  9. custom710 mg (79%) of the expected acid were collected

Sources & evidence

ORD record
ord-70a992d48da74f6ea1be99ec2d56d2cd
Source dataset
uspto-grants-1999_09
Patent number
US05952382

Reaction notes

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