Sodium Hydroxide → 10,11-Dihydro-2-methylsulfonyl-11-oxodibenzo[b,f]thiepin

HRID 35272ノート

反応式

HRID 35272 の反応式
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([S:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[CH2:18][C:19]([OH:21])=O)=[CH:7][CH:6]=1)(=[O:4])=[O:3].[OH-].[Na+]>>[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]2[S:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH2:18][C:19](=[O:21])[C:9]=2[CH:10]=1)(=[O:3])=[O:4]

参加物

3

反応物 2

HCID 14798Sodium HydroxideHCID 15729869HCID 15729869、化合物

生成物 1

HCID 1572986710,11-Dihydro-2-methylsulfonyl-11-oxodibenzo[b,f]thiepin

実験手順

A mixture of 1.0 g of 2-(4-methylsulfonylphenylthio)phenylacetic acid and 10 ml of polyphosphoric acid under nitrogen is stirred at 90°-100° C. for 2 hours. The reaction mixture is permitted to cool and then poured into 100 ml of an ice-water slurry. The aqueous solution is basified with 20% sodium hydroxide before being extracted with methylene chloride. The combined extracts are dried and then evaporated to dryness leaving an oil. The oil is chromatographed through a silica gel column with a 2% methanol in methylene chloride eluant. The chromatographed solution is evaporated to dryness providing 10,11-dihydro-2-methylsulfonyl-11-oxodibenzo[b,f]thiepin.

後処理

  1. temperatureto cool
  2. extractionbefore being extracted with methylene chloride
  3. customThe combined extracts are dried
  4. customevaporated to dryness
  5. customleaving an oil
  6. customThe oil is chromatographed through a silica gel column with a 2% methanol in methylene chloride eluant
  7. customThe chromatographed solution is evaporated to dryness

出典と根拠

ORDレコード
ord-017cd3fabbde49c595730d7e1bffeeda
出典データセット
uspto-grants-1988_08
特許番号
US04766143

反応ノート

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