6-Methoxy-isoquinoline 2-oxide hydrochloride → 1-Chloro-6-methoxyisoquinoline

HRID 1070556

反応式

HRID 1070556 の反応式
[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[CH:10]=[N+:9]([O-])[CH:8]=[CH:7]2>P(Cl)(Cl)(Cl)=O>[Cl:1][C:10]1[C:11]2[C:6](=[CH:5][C:4]([O:3][CH3:2])=[CH:13][CH:12]=2)[CH:7]=[CH:8][N:9]=1

参加物

3

反応物 1

HCID 223973326-Methoxy-isoquinoline 2-oxide hydrochloride

生成物 1

HCID 219010741-Chloro-6-methoxyisoquinoline

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

反応条件

温度
90 °C

実験手順

6-Methoxy-isoquinoline-N-oxide hydrochloride (1a, 85 g; 400 mmol) was carefully added in portions to phosphoryl chloride (550 mL) at a temperature of 90° C., after which the mixture was stirred for 6 h at 90° C. Excess of phosphoryl chloride was removed in vacuo. The remaining white solid was washed with water, filtered and dried in vacua. Yield: 68 g (88%); white solid; m.p. 72-74° C.; El-MS: 193 (M+).

後処理

  1. customExcess of phosphoryl chloride was removed in vacuo
  2. washThe remaining white solid was washed with water
  3. filtrationfiltered
  4. customdried in vacua

出典と根拠

ORDレコード
ord-f65656e336f847d098a261866c2b097a
出典データセット
uspto-grants-2005_06
特許番号
US06903107B1

関連ノート

読み込み中…