Potassium Hydroxide → HCID 10921070, compound

HRID 973436Notes

Reaction equation

HRID 973436 reaction equation
[OH-].[K+].[CH3:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](=[CH2:16])[C:12]([O:14]C)=[O:13]>O1CCCC1>[CH3:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](=[CH2:16])[C:12]([OH:14])=[O:13]

Participants

4

Reactant 2

HCID 14797Potassium HydroxideHCID 15052142HCID 15052142, compound

Product 1

HCID 10921070HCID 10921070, compoundYield 86.3%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

765 ml of an aqueous solution (0.33M) of potassium hydroxide were added to a solution of 21 g of the product of Step B in 1 liter of tetrahydrofuran and the mixture was stirred for 48 hours at ambient temperature. The tetrahydrofuran was evaporated off and the aqueous phase was cooled and acidified with 2N hydrochloric acid. Separation was carried out, then washing with water and drying to obtain 16.8 g of the product which was used as is for the following step. An analytical sample was prepared by hot and cold crystallization of 1.6 g of product from 30 ml of isopropyl ether to obtain 0.8 g of the product melting at 146° C.

Workup

  1. customThe tetrahydrofuran was evaporated off
  2. temperaturethe aqueous phase was cooled
  3. customSeparation
  4. washwashing with water
  5. customdrying

Sources & evidence

ORD record
ord-a5a338d0b7b043cea99ee832cacc78b4
Source dataset
uspto-grants-1991_11
Patent number
US05063225

Reaction notes

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