Dimethylformamide → HCID 21408360、化合物

HRID 2072545

反応式

HRID 2072545 の反応式
[C:1]1([C:7](=[O:16])[CH:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)Cl)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([S:20][CH2:21][C:22]([OH:24])=[O:23])(=O)N.[CH3:25][N:26](C=O)C>>[C:10]1([C:8]2[N:26]=[C:25]([CH:21]([SH:20])[C:22]([OH:24])=[O:23])[O:16][C:7]=2[C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

4

反応物 3

HCID 6228DimethylformamideHCID 95343Ethanone, 2-chloro-1,2-diphenyl-HCID 23423126(Carbamoylsulfanyl)acetic acid

生成物 1

HCID 21408360HCID 21408360、化合物

実験手順

23 g. of 1,2-diphenyl-2-chloroethanone is heated together with 18 g. of the ethyl ester of carbamoylmercaptoacetic acid in 150 ml. of absolute DMF for 3 hours to 70°. Then, the DMF is removed, and the residue, containing the ethyl ester of N-(1,2-diphenyl-2-oxoethyl)-carbamoylmercaptoacetic acid, is refluxed for 5 hours with a mixture of 100 g. of POCl3 and 200 ml. of benzene. The mixture is then evaporated under reduced pressure and the residue is purified by chromatography on silica gel, thus obtaining the ethyl ester of 4,5-diphenyl-2-oxazolyl-mercaptoacetic acid, m.p. 54°-56°.

後処理

  1. customThen, the DMF is removed
  2. additionthe residue, containing the ethyl ester of N-(1,2-diphenyl-2-oxoethyl)-carbamoylmercaptoacetic acid
  3. temperatureis refluxed for 5 hours with a mixture of 100 g
  4. customThe mixture is then evaporated under reduced pressure
  5. customthe residue is purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-156f575e82c1420193bc723d5471a5db
出典データセット
uspto-grants-1977_09
特許番号
US04051250

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