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2-Aminothiazole → (E)-4-cyclopentyl-2-(4-methanesulfonyl-3-trifluoromethyl-phenyl)-but-2-enoic acid thiazol-2-ylamide

HRID 276233
ノート
印刷プレビュー

反応式

HRID 276233 の反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.BrN1C(=O)CCC1=O.[CH:28]1([CH2:33]/[CH:34]=[C:35](\[C:39]2[CH:44]=[CH:43][C:42]([S:45]([CH3:48])(=[O:47])=[O:46])=[C:41]([C:49]([F:52])([F:51])[F:50])[CH:40]=2)/[C:36]([OH:38])=O)[CH2:32][CH2:31][CH2:30][CH2:29]1.[NH2:53][C:54]1[S:55][CH:56]=[CH:57][N:58]=1>C(Cl)Cl>[S:55]1[CH:56]=[CH:57][N:58]=[C:54]1[NH:53][C:36](=[O:38])/[C:35](/[C:39]1[CH:44]=[CH:43][C:42]([S:45]([CH3:48])(=[O:46])=[O:47])=[C:41]([C:49]([F:52])([F:50])[F:51])[CH:40]=1)=[CH:34]/[CH2:33][CH:28]1[CH2:32][CH2:31][CH2:30][CH2:29]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 21552-AminothiazoleHCID 11776TriphenylphosphineHCID 67184N-bromobutanimideHCID 67483112(E)-4-cyclopentyl-2-[4-(methanesulfonyl)-3-(trifluoromethyl)-phenyl)-but-2-enoic acid

生成物 1

HCID 52946400(E)-4-cyclopentyl-2-(4-methanesulfonyl-3-trifluoromethyl-phenyl)-but-2-enoic acid thiazol-2-ylamide収率 16%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of triphenylphosphine (550 mg, 2.1 mmol) in methylene chloride (25 mL) was cooled to 0° C. and then treated with N-bromosuccinimide (374 mg, 2.1 mmol). The reaction mixture was stirred at 0° C. for 30 min and then treated with a solution of (E)-4-cyclopentyl-2-[4-(methanesulfonyl)-3-(trifluoromethyl)-phenyl)-but-2-enoic acid (395 mg, 1.05 mmol) in methylene chloride (5 mL). The clear solution was stirred for 15 min at 0° C. and then allowed to warm to 25° C. where it was stirred for 1.5 h. The reaction mixture was then treated with 2-aminothiazole (320 mg, 3.2 mmol), and the resulting suspension was stirred at 25° C. over the weekend. The reaction mixture was concentrated in vacuo to remove methylene chloride, and the residue was diluted with ethyl acetate (50 mL) and a 1N aqueous hydrochloric acid solution (50 mL). The two layers were separated, and the aqueous layer was extracted with ethyl acetate (1×30 mL). The combined organic extracts were successively washed with a saturated aqueous sodium bicarbonate solution (2×50 mL) and a saturated aqueous sodium chloride solution (1×100 mL). The organic layer was then dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. Biotage chromatography (FLASH 40M, Silica, 1/1 hexanes/ethyl acetate) afforded the (E)-4-cyclopentyl-2-(4-methanesulfonyl-3-trifluoromethyl-phenyl)-but-2-enoic acid thiazol-2-ylamide (77 mg, 16%) as an amorphous solid: EI-HRMS m/e calcd for C20H21F3N2O3S2 (M+) 458.0946, found 458.0946.

後処理

  1. stirringThe clear solution was stirred for 15 min at 0° C.
  2. temperatureto warm to 25° C. where it
  3. stirringwas stirred for 1.5 h
  4. stirringthe resulting suspension was stirred at 25° C. over the weekend
  5. concentrationThe reaction mixture was concentrated in vacuo
  6. customto remove methylene chloride
  7. additionthe residue was diluted with ethyl acetate (50 mL)
  8. customThe two layers were separated
  9. extractionthe aqueous layer was extracted with ethyl acetate (1×30 mL)
  10. washThe combined organic extracts were successively washed with a saturated aqueous sodium bicarbonate solution (2×50 mL)
  11. dry with materialThe organic layer was then dried over anhydrous magnesium sulfate
  12. filtrationfiltered
  13. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9a8b9fa251a541008571054d42f6da7a
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06353111B1

反応ノート

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