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Triethylamine → 3,3,3-Trifluoro-N-[4-methyl-2-(pyridin-3-yl)-1,3-thiazol-5-yl]propanamide

HRID 1182778
ノート
印刷プレビュー

反応式

HRID 1182778 の反応式
[CH3:1][C:2]1[N:3]=[C:4]([C:8]2[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=2)[S:5][C:6]=1[NH2:7].C(N(CC)CC)C.[F:21][C:22]([F:28])([F:27])[CH2:23][C:24](Cl)=[O:25]>C1COCC1>[F:21][C:22]([F:28])([F:27])[CH2:23][C:24]([NH:7][C:6]1[S:5][C:4]([C:8]2[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=2)=[N:3][C:2]=1[CH3:1])=[O:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 27833433,3,3-Trifluoropropionyl chlorideHCID 666453454-Methyl-2-(pyridin-3-yl)-1,3-thiazole-5-amine

生成物 1

HCID 534829763,3,3-Trifluoro-N-[4-methyl-2-(pyridin-3-yl)-1,3-thiazol-5-yl]propanamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

286 mg (1.49 mmol) of 4-methyl-2-(pyridin-3-yl)-1,3-thiazole-5-amine were dissolved in THF, 0.52 ml of triethylamine was added, and 263 mg of trifluoropropionyl chloride were added while cooling with an ice bath. The mixture was stirred at room temperature overnight and then concentrated. Ethyl acetate, saturated sodium chloride solution and aqueous phosphate buffer pH=7 were added to the residue, the aqueous phase was extracted twice with ethyl acetate, and the combined organic phases were dried over Na2SO4 and concentrated. The residue was purified by chromatography (silica gel, cyclohexane, acetone).

後処理

  1. temperaturewhile cooling with an ice bath
  2. concentrationconcentrated
  3. additionEthyl acetate, saturated sodium chloride solution and aqueous phosphate buffer pH=7 were added to the residue
  4. extractionthe aqueous phase was extracted twice with ethyl acetate
  5. dry with materialthe combined organic phases were dried over Na2SO4
  6. concentrationconcentrated
  7. customThe residue was purified by chromatography (silica gel, cyclohexane, acetone)

出典と根拠

ORDレコード
ord-2539c85d0839477897a8a5ac17898c13
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08664229B2

反応ノート

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