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Water → HCID 52913378、化合物

HRID 540798
ノート
印刷プレビュー

反応式

HRID 540798 の反応式
[NH2:1][C:2]1([C:6]2[CH:7]=[C:8]([C:12]3[CH:16]=[C:15]([O:17][C:18]4[CH:23]=[CH:22][C:21]([C:24]([F:27])([F:26])[F:25])=[CH:20][CH:19]=4)[N:14]([CH2:28][C:29]([N:31]([CH3:33])[CH3:32])=[O:30])[N:13]=3)[CH:9]=[CH:10][CH:11]=2)[CH2:5][O:4][CH2:3]1.C(N(CC)CC)C.[F:41][C:42]([F:49])([F:48])[CH2:43][S:44](Cl)(=[O:46])=[O:45].O>C(Cl)Cl>[F:27][C:24]([F:25])([F:26])[C:21]1[CH:20]=[CH:19][C:18]([O:17][C:15]2[N:14]([CH2:28][C:29]([N:31]([CH3:33])[CH3:32])=[O:30])[N:13]=[C:12]([C:8]3[CH:9]=[CH:10][CH:11]=[C:6]([C:2]4([NH:1][S:44]([CH2:43][C:42]([F:49])([F:48])[F:41])(=[O:46])=[O:45])[CH2:5][O:4][CH2:3]4)[CH:7]=3)[CH:16]=2)=[CH:23][CH:22]=1
参加物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 962WaterHCID 8471TriethylamineHCID 742422,2,2-Trifluoroethanesulfonyl chlorideHCID 69933247HCID 69933247、化合物

生成物 1

HCID 52913378HCID 52913378、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A stirred solution of 2-{3-[3-(3-aminooxetan-3-yl)phenyl]-5-(4-trifluoromethylphenoxy)-1H-pyrazol-1-yl}-N,N-dimethylacetamide (46 mg, 0.10 mmol) in 1 mL of CH2Cl2 was cooled in an ice bath. Triethylamine (0.021 mL, 0.15 mmol) was added, followed by trifluoroethylsulfonyl chloride (0.013 mL, 0.12 mmol), and the mixture was stirred for 30 min. Water was added and the mixture was extracted with CH2Cl2. The combined organic phases were washed with water and brine, then dried over Na2SO4, filtered, and the solvent was removed under reduced pressure. The residue was purified on a C18 reverse phase column using a gradient elution of 20-70% CH3CN:H2O with 0.1% TFA over 20 min at 20 mL/min. Fractions containing pure product were combined and the solvents were removed under reduced pressure to give 2-[5-(4-trifluoromethylphenoxy)-3-(3-{3-[(2,2,2-trifluoroethylsulfonyl)amino]oxetan-3-yl}phenyl)-1H-pyrazol-1-yl]-N,N-dimethylacetamide as a foam. Calcd (M+1)+: 607.1444. Found: 607.1468. 1H NMR (400 MHz, CDCl3) δ 7.75 (m, 2H), 7.64 (d, J=7, 2H), 7.44 (t, J=7, 1H), 7.35 (m, 2H), 7.28 (s, 1H), 6.38 (s, 1H), 6.04 (s, 1H), 5.04 (d, J=7, 2H), 4.98 (d, J=7, 2H), 4.94 (s, 2H), 3.09 (s, 3H), 2.97 (overlapping s and q, 5H).

後処理

  1. extractionthe mixture was extracted with CH2Cl2
  2. washThe combined organic phases were washed with water and brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customthe solvent was removed under reduced pressure
  6. customThe residue was purified on a C18 reverse phase column
  7. washa gradient elution of 20-70% CH3CN
  8. waitH2O with 0.1% TFA over 20 min at 20 mL/min
  9. additionFractions containing pure product
  10. customthe solvents were removed under reduced pressure

出典と根拠

ORDレコード
ord-5a9008afed1d4b62b35c860f67778408
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871796B2

反応ノート

読み込み中…

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