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

HRID 542883노트

반응식

HRID 542883 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fca27d4039b14be8a4308d8fcfcf2248
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04659727

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