Sodium methanethiolate → 6-Isoquinolinol, 7-methyl- (9CI)

HRID 228875ノート

反応式

HRID 228875 の反応式
C[O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[CH3:13])[CH:9]=[N:8][CH:7]=[CH:6]2.C[S-].[Na+]>CN(C)C=O>[OH:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[CH3:13])[CH:9]=[N:8][CH:7]=[CH:6]2

参加物

4

反応物 2

HCID 4378561Sodium methanethiolateHCID 230784386-Methoxy-7-methylisoquinoline

生成物 1

HCID 1357421666-Isoquinolinol, 7-methyl- (9CI)収率 9.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
160 °C

実験手順

6-Methoxy-7-methylisoquinoline (239 mg) and sodium thiomethoxide (1.58 g) were suspended in N,N-dimethylformamide (12 ml), and the suspension was stirred at 160° C. for 2 hr. The reaction solution was cooled to room temperature, the reaction solution was then filtered, and the solvent was removed from the filtrate by distillation under the reduced pressure. The residue was purified by thin layer chromatography using chloroform-methanol to give 6-hydroxy-7-methylisoquinoline (21 mg, yield 1%).

後処理

  1. temperatureThe reaction solution was cooled to room temperature
  2. filtrationthe reaction solution was then filtered
  3. customthe solvent was removed from the filtrate by distillation under the reduced pressure
  4. customThe residue was purified by thin layer chromatography

出典と根拠

ORDレコード
ord-59963b43ab36432bae428be123756b9a
出典データセット
uspto-grants-2009_07
特許番号
US07560558B2

反応ノート

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