Phosphorus oxychloride → HCID 84687221, compound

HRID 1470461Notes

Reaction equation

HRID 1470461 reaction equation
O[C:2]1[C:11]2[C:6](=[C:7]([CH3:12])[CH:8]=[CH:9][CH:10]=2)[C:5]([C:13]([OH:15])=[O:14])=[CH:4][N:3]=1.O=P(Cl)(Cl)[Cl:18]>>[Cl:18][C:2]1[C:11]2[C:6](=[C:7]([CH3:12])[CH:8]=[CH:9][CH:10]=2)[C:5]([C:13]([OH:15])=[O:14])=[CH:4][N:3]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 1784239111-Hydroxy-5-methylisoquinolin-4-carboxylic acid

Product 1

HCID 84687221HCID 84687221, compoundYield 86%

Procedure

A stirred solution of 1-hydroxy-5-methylisoquinolin-4-carboxylic acid (Intermediate-9) (600 mg, 3 mmol) in POCl3 (10 mL) was heated to 100° C. for 40-50 min. The reaction mixture was poured into ice-water, extracted with CH2Cl2 (2×100 mL), washed with water (2×100 mL), dried over Na2SO4, filtered and evaporated to give the desired compound (550 mg, 86%).

Workup

  1. extractionextracted with CH2Cl2 (2×100 mL)
  2. washwashed with water (2×100 mL)
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customevaporated

Sources & evidence

ORD record
ord-8475d74a08754674b37cbfb0b4f60635
Source dataset
uspto-grants-2015_04
Patent number
US09006442B2

Reaction notes

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