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Sodium Chloride → Rac-5-[3-(4-fluoro-phenyl)-5-hydroxymethyl-isoxazol-4-ylmethoxy]-2-methyl-2h-pyrazole-3-carboxylic acid (tetrahydro-furan-3-yl)-amide

HRID 1695437
ノート
印刷プレビュー

反応式

HRID 1695437 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:12]([CH2:13][O:14][C:15]3[CH:16]=[C:17]([C:21]([OH:23])=O)[N:18]([CH3:20])[N:19]=3)=[C:11]([CH2:24][OH:25])[O:10][N:9]=2)=[CH:4][CH:3]=1.O.ON1C2C=CC=CC=2N=N1.C(N(C(C)C)C(C)C)C.[NH2:46][CH:47]1[CH2:51][CH2:50][O:49][CH2:48]1.[Cl-].[Na+]>C1COCC1>[O:49]1[CH2:50][CH2:51][CH:47]([NH:46][C:21]([C:17]2[N:18]([CH3:20])[N:19]=[C:15]([O:14][CH2:13][C:12]3[C:8]([C:5]4[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=4)=[N:9][O:10][C:11]=3[CH2:24][OH:25])[CH:16]=2)=[O:23])[CH2:48]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 5234Sodium ChlorideHCID 81531DiisopropylethylamineHCID 27960291-Hydroxybenzotriazole hydrateHCID 3365553Oxolan-3-amineHCID 666438625-[3-(4-fluoro-phenyl)-5-hydroxymethyl-isoxazol-4-ylmethoxy]-2-methyl-2H-pyrazole-3-carboxylic acid

生成物 1

HCID 59568389
Rac-5-[3-(4-fluoro-phenyl)-5-hydroxymethyl-isoxazol-4-ylmethoxy]-2-methyl-2h-pyrazole-3-carboxylic acid (tetrahydro-furan-3-yl)-amide
収率 50%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 5-[3-(4-fluoro-phenyl)-5-hydroxymethyl-isoxazol-4-ylmethoxy]-2-methyl-2H-pyrazole-3-carboxylic acid (100 mg, 0.29 mmol) in THF (10 mL) was added 1-hydroxybenzotriazole hydrate (45.0 mg, 0.29 mmol), N-ethyldiisopropylamine (126 μL, 0.76 mmol), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimidazole hydrochloride (56.3 mg, 0.29 mmol) and rac-3-aminotetrahydrofuran (25.1 mg, 0.29 mmol) and the resulting mixture stirred overnight at room temperature. The reaction mixture was then poured into aqueous sodium chloride (saturated) and the mixture was extracted with ethyl acetate. The combined organic layers were then washed with water and saturated sodium hydrogen carbonate solution and then dried over sodium sulfate, filtered and evaporated. Concentration and purification by chromatography (silica, dichloromethane:methanol=99:1 to 95:5) afforded the title compound (60 mg, 50%) as a white solid. MS: m/e=415.1 [M−H]−.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe combined organic layers were then washed with water and saturated sodium hydrogen carbonate solution
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. concentrationConcentration and purification by chromatography (silica, dichloromethane:methanol=99:1 to 95:5)

出典と根拠

ORDレコード
ord-9ec924369fb543bab8d7916fdb0d2f97
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163728B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート