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Triethylamine → 1-(4-Trifluoromethylpyrimidin-5-yl)-1-(4-methoxypyrimidin-5-yl)-1-trimethylacetoxymethane

HRID 861392
ノート
印刷プレビュー

反応式

HRID 861392 の反応式
[CH3:1][C:2]([CH3:7])([CH3:6])[C:3](Cl)=[O:4].[F:8][C:9]([F:27])([F:26])[C:10]1[C:15]([CH:16]([C:18]2[C:19]([O:24][CH3:25])=[N:20][CH:21]=[N:22][CH:23]=2)[OH:17])=[CH:14][N:13]=[CH:12][N:11]=1.C(N(CC)CC)C.CN(C1C=CC=CN=1)C>C1(C)C=CC=CC=1.C([O-])(O)=O.[Na+]>[F:27][C:9]([F:8])([F:26])[C:10]1[C:15]([CH:16]([C:18]2[C:19]([O:24][CH3:25])=[N:20][CH:21]=[N:22][CH:23]=2)[O:17][C:3](=[O:4])[C:2]([CH3:7])([CH3:6])[CH3:1])=[CH:14][N:13]=[CH:12][N:11]=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 4

HCID 8471TriethylamineHCID 218852-DimethylaminopyridineHCID 62493Pivaloyl chlorideHCID 197028001-(4-Trifluoromethylpyrimidin-5-yl)-1-(4-methoxypyrimidin-5-yl)methanol

生成物 1

HCID 676303761-(4-Trifluoromethylpyrimidin-5-yl)-1-(4-methoxypyrimidin-5-yl)-1-trimethylacetoxymethane収率 80.1%

試薬・触媒・溶媒 2

HCID 1140
Toluene
溶媒
HCID 516892Sodium Bicarbonate溶媒

実験手順

Trimethylacetyl chloride (36 μl, 35.1 mg, 0.28 mmol, 3.2 equivalent) was added via syringe to a solution of 1-(4-trifluoromethylpyrimidin-5-yl)-1-(4-methoxypyrimidin-5-yl)methanol (25.1 mg, 0.0877 mmol), triethylamine (70 μl, 50.5 mg, 0.50 mmol, 5.7 equivalents) and dimethylaminopyridine (DMAP) (cat.) in toluene (5 ml) and the solution heated to reflux for 2 hours. The solution was cooled, diluted with NaHCO3 (sat.), and extracted with EtOAc (3 times). The combined extracts were washed with brine (sat.), dried (MgSO4), filtered and concentrated in vacuo. Preparative thin layer chromatography (SiO2 ; hexane/EtOAc, 1:1) gave 26 mg of 1-(4-trifluoromethylpyrimidin-5-yl)-1-(4-methoxypyrimidin-5-yl)-1-trimethylacetoxymethane as a solid.

後処理

  1. temperaturethe solution heated
  2. temperatureto reflux for 2 hours
  3. temperatureThe solution was cooled
  4. extractionextracted with EtOAc (3 times)
  5. washThe combined extracts were washed with brine (sat.)
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-975db8ccb89b43608e1fa2bb8d2afb8f
出典データセット
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05714438

反応ノート

読み込み中…

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