Diethyl Ether → Methyl 5-phenyl-2-{[3-(trifluoromethyl)phenyl]amino}4-thiazolecarboxylate

HRID 359260노트

반응식

HRID 359260 반응식
[C:1]1([C:7]2[S:11][C:10](Cl)=[N:9][C:8]=2[C:13]([O:15][CH3:16])=[O:14])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH2:17][C:18]1[CH:19]=[C:20]([C:24]([F:27])([F:26])[F:25])[CH:21]=[CH:22][CH:23]=1.C(OCC)C>O>[C:1]1([C:7]2[S:11][C:10]([NH:17][C:18]3[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([F:25])([F:26])[F:27])[CH:19]=3)=[N:9][C:8]=2[C:13]([O:15][CH3:16])=[O:14])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 73753-(Trifluoromethyl)anilineHCID 12821997Methyl 2-chloro-5-phenyl-4-thiazolecarboxylate

생성물 1

HCID 20064764Methyl 5-phenyl-2-{[3-(trifluoromethyl)phenyl]amino}4-thiazolecarboxylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A reaction vessel was charged with 2.8 g of methyl 5-phenyl-2-chloro-4-thiazolecarboxylate and 9.7 g of meta-aminobenzotrifluoride. The reaction mixture was stirred overnight and then heated and stirred at 150° C. for about 6 hours during which time a crystalline solid appeared. The mixture was treated with ethyl ether and water. The ether extract was dried with magnesium sulfate and concentrated. The residue was crystallized from anhydrous ethyl ether to provide a white amorphous powder (m.p. 147°-149° C.) identified in Table I.

후처리

  1. temperatureheated
  2. stirringstirred at 150° C. for about 6 hours during which time a crystalline solid
  3. extractionThe ether extract
  4. dry with materialwas dried with magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was crystallized from anhydrous ethyl ether

출처 및 근거

ORD 기록
ord-8955d1581eff4c428c6e2f5fe2a66864
출처 데이터셋
uspto-grants-1991_03
특허 번호
US05000775

반응 노트

불러오는 중…