Phosphorus sulfide (P2S5) → 6,7-Dimethoxyquinoline-4(1H)-thione

HRID 387840

反応式

HRID 387840 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[NH:9][CH:8]=[CH:7][C:6]2=O.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:17].C(=O)(O)[O-].[Na+]>COCCOCCOC>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[NH:9][CH:8]=[CH:7][C:6]2=[S:17]

参加物

5

反応物 3

HCID 14817Phosphorus sulfide (P2S5)HCID 4596116,7-Dimethoxy-4-hydroxyquinolineHCID 516892Sodium Bicarbonate

生成物 1

HCID 229368096,7-Dimethoxyquinoline-4(1H)-thione収率 74%

試薬・触媒・溶媒 1

HCID 8150Diglyme溶媒

反応条件

温度
80 °C

実験手順

After suspending the 6,7-dimethoxy-1H-quinolin-4-one (10.3 g, 50.0 mmol) described in WO9717329, phosphorus pentasulfide (26.7 g, 60.0 mmol) and sodium bicarbonate (26.7 g, 318 mmol) in diglyme (diethyleneglycol dimethyl ether) (100 ml), the suspension was heated and stirred at 80° C. for 2 hours. The reaction solution was returned to room temperature and poured into ice water (1000 ml), and the precipitated crystals were filtered out, washed with water and blow-dried to obtain the title compound (8.19 g, 37.0 mmol, 74%) as yellow crystals.

後処理

  1. temperaturethe suspension was heated
  2. customwas returned to room temperature
  3. filtrationthe precipitated crystals were filtered out
  4. washwashed with water
  5. customblow-dried

出典と根拠

ORDレコード
ord-de954c1791554d049741d22c2fa7a9ff
出典データセット
uspto-grants-2013_02
特許番号
US08372981B2

関連ノート

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