Pyridinium chloride → HCID 13290010、化合物

HRID 370942ノート

反応式

HRID 370942 の反応式
[Cl:1][C:2]1[C:3]([O:14]C)=[CH:4][C:5]2[CH:9]=[C:8]([CH2:10][CH3:11])[S:7][C:6]=2[C:12]=1[Cl:13].Cl.N1C=CC=CC=1>>[Cl:1][C:2]1[C:3]([OH:14])=[CH:4][C:5]2[CH:9]=[C:8]([CH2:10][CH3:11])[S:7][C:6]=2[C:12]=1[Cl:13]

参加物

3

反応物 2

HCID 10176127Pyridinium chlorideHCID 13290009HCID 13290009、化合物

生成物 1

HCID 13290010HCID 13290010、化合物収率 73.7%

実験手順

A mixture of 2.15 g of 6,7-dichloro-2-ethyl-5-methoxybenzo[b]thiophene and 15 g of pyridine hydrochloride is stirred at 170°-180° for 90 min. The mixture is cooled, triturated with water and extracted three times with dichloromethane. The combined organic extracts are washed with water, dried over anhydrous magnesium sulfate and concentrated in vacuo to an oily residue. Purification by column chromatography (silica gel-etherpentane 50:50) affords 1.5 g of 6,7-dichloro-2-ethyl-5-hydroxybenzo[b]thiophene as off-white crystals, mp 69°-70°.

後処理

  1. temperatureThe mixture is cooled
  2. customtriturated with water
  3. extractionextracted three times with dichloromethane
  4. washThe combined organic extracts are washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo to an oily residue
  7. customPurification by column chromatography (silica gel-etherpentane 50:50)

出典と根拠

ORDレコード
ord-4181b812fa074a819138e9d868166665
出典データセット
uspto-grants-1985_07
特許番号
US04528399

反応ノート

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