Pyridinium chloride → HCID 13290070、化合物

HRID 652682ノート

反応式

HRID 652682 の反応式
[Cl:1][C:2]1[C:3]([O:15]C)=[CH:4][C:5]2[CH:9]=[C:8]([CH2:10][CH2:11][CH3:12])[S:7][C:6]=2[C:13]=1[Cl:14].Cl.N1C=CC=CC=1>O>[Cl:1][C:2]1[C:3]([OH:15])=[CH:4][C:5]2[CH:9]=[C:8]([CH2:10][CH2:11][CH3:12])[S:7][C:6]=2[C:13]=1[Cl:14]

参加物

4

反応物 2

HCID 10176127Pyridinium chlorideHCID 139528716,7-Dichloro-5-methoxy-2-n-propylbenzo[b]thiophene

生成物 1

HCID 13290070HCID 13290070、化合物収率 56.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 29 g of 6,7-dichloro-5-methoxy-2-n-propylbenzo[b]thiophene and 280 g of pyridine hydrochloride is heated at 190° for 5 hrs and allowed to cool. The reaction mixture is poured into 300 ml of water and extracted with three 33-ml portions of ether. The ether extracts are washed with 500 ml of 2N hydrochloric acid, water, dried over anhydrous magnesium sulfate-charcoal, filtered and evaporated to give an oil. Crystallization of the oil with hexane followed by recrystallization from hexane give 15.5 g of 6,7-dichloro-5-hydroxy-2-n-propylbenzo[b]thiophene, mp 50°-51°.

後処理

  1. temperatureis heated at 190° for 5 hrs
  2. temperatureto cool
  3. extractionextracted with three 33-ml portions of ether
  4. washThe ether extracts are washed with 500 ml of 2N hydrochloric acid, water
  5. dry with materialdried over anhydrous magnesium sulfate-charcoal
  6. filtrationfiltered
  7. customevaporated
  8. customto give an oil
  9. customCrystallization of the oil with hexane
  10. customfollowed by recrystallization from hexane

出典と根拠

ORDレコード
ord-2f4b9b02660d408aa071de6713ffa792
出典データセット
uspto-grants-1987_06
特許番号
US04672138

反応ノート

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