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

HRID 853363

반응식

HRID 853363 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8150Diglyme용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9b0baa9734fd4552981be5825d67b46d
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253286B2

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