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Ethanol → 3-[(2-Oxo-2-phenylethyl)thio]-5-(trifluoromethyl)benzoic acid

HRID 1606761
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HRID 1606761 반응식
[SH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1)[C:5]([OH:7])=[O:6].[OH-].[Na+].Cl[CH2:18][C:19]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[O:20].C(O)C>O>[CH2:18]([S:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([C:11]([F:12])([F:13])[F:14])[CH:10]=1)[C:5]([OH:7])=[O:6])[C:19]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[O:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 702EthanolHCID 107572-ChloroacetophenoneHCID 14798Sodium HydroxideHCID 21542284HCID 21542284, 화합물

생성물 1

HCID 215444803-[(2-Oxo-2-phenylethyl)thio]-5-(trifluoromethyl)benzoic acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1.33 g. (6 m moles) of 3-mercapto-5-trifluoromethylbenzoic acid, 12 ml. of 1N sodium hydroxide solution and 930 mg. (6 m moles) of α-chloroacetophenone in 20 ml. of ethanol is allowed to stir at room temperature for 1 hour. The reaction mixture is diluted with water, extracted with ether and the resulting aqueous phase acidified with 12N hydrochloric acid. The light yellow oil which separates gradually crystallizes and is filtered, 1.8 g., m.p. 135°-150° C. A sample is sublimed at 165° C. and 0.05 mm pressure, m.p. 153°-155° C.

후처리

  1. additionA mixture of 1.33 g
  2. extractionextracted with ether
  3. customThe light yellow oil which separates gradually crystallizes
  4. filtrationis filtered
  5. customis sublimed at 165° C.

출처 및 근거

ORD 기록
ord-e36e3b0729484a2ea375cfaa31e9e3ec
출처 데이터셋
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03953595

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