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

HRID 867470노트

반응식

HRID 867470 반응식
[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]

참가 물질

3

반응물 2

HCID 14798Sodium HydroxideHCID 15729869HCID 15729869, 화합물

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ad9f4a329b9d49bb9722f5c66efbce7e
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04775683

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