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

HRID 853363

反応式

HRID 853363 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-9b0baa9734fd4552981be5825d67b46d
出典データセット
uspto-grants-2007_08
特許番号
US07253286B2

関連ノート

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