2-Aminothiazole → 1,1-Bis(phenylsulphonyl)-2-(thiazol-2-ylamino)ethene

HRID 542883ノート

反応式

HRID 542883 の反応式
[NH2:1][C:2]1[S:3][CH:4]=[CH:5][N:6]=1.C(O[CH:10]=[C:11]([S:21]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)(=[O:23])=[O:22])[S:12]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)(=[O:14])=[O:13])C>CC(N(C)C)=O>[C:15]1([S:12]([C:11]([S:21]([C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)(=[O:23])=[O:22])=[CH:10][NH:1][C:2]2[S:3][CH:4]=[CH:5][N:6]=2)(=[O:13])=[O:14])[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

参加物

4

反応物 2

HCID 21552-AminothiazoleHCID 124009381,1-Bis(phenylsulphonyl)-2-ethoxyethene

生成物 1

HCID 202074261,1-Bis(phenylsulphonyl)-2-(thiazol-2-ylamino)ethene収率 44.3%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

A solution of 2-aminothiazole (0.5 g) and 2-ethoxy-1,1-bis(phenylsulphonyl)ethene (1.76 g) in dimethylacetamide (20 ml) was heated at reflux for 3.5 hours. The solution was cooled and poured onto ice (200 g) and then the resulting buff precipitate was filtered off, washed with water and dried in vacuo over phosphorous pentoxide. Recrystallisation from ethyl acetate gave 1,1-bis(phenylsulphonyl)-2-(thiazol-2-ylamino)ethene (0.9 g), m.p. 189°-191° C.

後処理

  1. temperatureat reflux for 3.5 hours
  2. temperatureThe solution was cooled
  3. additionpoured onto ice (200 g)
  4. filtrationthe resulting buff precipitate was filtered off
  5. washwashed with water
  6. dry with materialdried in vacuo over phosphorous pentoxide
  7. customRecrystallisation from ethyl acetate

出典と根拠

ORDレコード
ord-fca27d4039b14be8a4308d8fcfcf2248
出典データセット
uspto-grants-1987_04
特許番号
US04659727

反応ノート

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