Phosphorus oxychloride → HCID 84687221、化合物

HRID 1470461ノート

反応式

HRID 1470461 の反応式
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

参加物

3

反応物 2

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

生成物 1

HCID 84687221HCID 84687221、化合物収率 86%

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-8475d74a08754674b37cbfb0b4f60635
出典データセット
uspto-grants-2015_04
特許番号
US09006442B2

反応ノート

読み込み中…