Diethyl Ether → HCID 12837902, 화합물

HRID 1855767노트

반응식

HRID 1855767 반응식
[C:1]([S:4][CH2:5][C:6]([NH2:8])=[O:7])(=[O:3])[CH3:2].[C:9]1([CH2:15][C:16](Cl)=[O:17])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.CCOCC>S(=O)(=O)(O)O.CCCCCC>[C:9]1([CH2:15][C:16]([NH:8][C:6](=[O:7])[CH2:5][S:4][C:1](=[O:3])[CH3:2])=[O:17])[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

6

반응물 3

HCID 3283Diethyl EtherHCID 7679Phenylacetyl chlorideHCID 51082772-(Acetylthio)acetamide

생성물 1

HCID 12837902HCID 12837902, 화합물

시약·촉매·용매 2

HCID 1118Sulfuric Acid촉매HCID 8058Hexane용매

실험 절차

A reaction mixture comprising 6.65 g. (0.05 mole) of 2-(acetylthio)acetamide, 10 ml. of 2-phenylacetyl chloride, and 1 drop of sulfuric acid was heated in a steam bath for 0.5 hour, and then allowed to stand overnight at room temperature, after which it solidified. There was then added 50 ml. of ether and 20 ml. of hexane, followed by stirring for 10 minutes and then filtering. A yield of 8.5 g. of a tan solid was obtained, which was then chromatographed on 100 g. of silica gel, eluting with 5% ether in dichloromethane, followed by concentration to dryness. The solid was suspended in 60 ml. of ethanol and stirred in an ice bath for 1 hour. The product of white crystals, m.p. 153°-155° C., was obtained in a 5.6 g. yield.

후처리

  1. additionThere was then added 50 ml
  2. filtrationfiltering
  3. customof a tan solid was obtained
  4. customwhich was then chromatographed on 100 g
  5. washof silica gel, eluting with 5% ether in dichloromethane
  6. concentrationfollowed by concentration to dryness
  7. stirringof ethanol and stirred in an ice bath for 1 hour
  8. customThe product of white crystals, m.p. 153°-155° C., was obtained in a 5.6 g
  9. customyield

출처 및 근거

ORD 기록
ord-82908aee71f149ad99658928b8def460
출처 데이터셋
uspto-grants-1980_08
특허 번호
US04216160

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