Diethyl Ether → HCID 12837902、化合物

HRID 1855767ノート

反応式

HRID 1855767 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 12837902HCID 12837902、化合物

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid触媒HCID 8058Hexane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-82908aee71f149ad99658928b8def460
出典データセット
uspto-grants-1980_08
特許番号
US04216160

反応ノート

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