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2,2,2-Trifluoroethanol → HCID 59347045、化合物

HRID 1009128
ノート
印刷プレビュー

反応式

HRID 1009128 の反応式
[H-].[Na+].[CH2:3]([OH:8])[C:4]([F:7])([F:6])[F:5].Cl[C:10]1[CH:15]=[C:14]([CH2:16][C@H:17]2[C@@H:21]([CH2:22][OH:23])[O:20][C:19]([CH3:25])([CH3:24])[N:18]2[C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])[CH:13]=[CH:12][N:11]=1>CN1C(=O)CCC1.CCOC(C)=O>[OH:23][CH2:22][C@H:21]1[O:20][C:19]([CH3:24])([CH3:25])[N:18]([C:26]([O:28][C:29]([CH3:31])([CH3:32])[CH3:30])=[O:27])[C@H:17]1[CH2:16][C:14]1[CH:15]=[CH:10][N:11]=[C:12]([O:8][CH2:3][C:4]([F:7])([F:6])[F:5])[CH:13]=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 3

HCID 64092,2,2-TrifluoroethanolHCID 24758Sodium hydrideHCID 59347033(4S,5S)-Tert-butyl 4-((2-chloropyridin-4-yl)methyl)-5-(hydroxymethyl)-2,2-dimethyloxazolidine-3-carboxylate

生成物 1

HCID 59347045HCID 59347045、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒
HCID 13387
N-methyl-2-pyrrolidone
溶媒

反応条件

温度
0 °C

実験手順

NaH (60% by weight in mineral oil) (0.672 g, 16.8 mmol) was added carefully to trifluoroethanol (20.0 ml, 276 mmol) cooled at 0° C. and then stirred at RT for 30 minutes. The resulting solution is added to (4S,5S)-tert-butyl 4-((2-chloropyridin-4-yl)methyl)-5-(hydroxymethyl)-2,2-dimethyloxazolidine-3-carboxylate (0.400 g, 1.12 mmol) dissolved in 10 mL of NMP and the resulting solution was microwaved for 30 minutes fixed at 180° C. The reaction was diluted with EtOAc and washed repeatedly with water. The combined aqueous layers were back extracted with EtOAc and the combined organic layers were washed with water, brine, dried over sodium sulfate and concentrated. The product was purified by silica gel chromatography (2:1 to 1:1 Hexanes/EtOAc) to afford the title compound. MS m/z: 421.3 (100%, M+1).

後処理

  1. customthe resulting solution was microwaved for 30 minutes
  2. customfixed at 180° C
  3. washwashed repeatedly with water
  4. extractionThe combined aqueous layers were back extracted with EtOAc
  5. washthe combined organic layers were washed with water, brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated
  8. customThe product was purified by silica gel chromatography (2:1 to 1:1 Hexanes/EtOAc)

出典と根拠

ORDレコード
ord-67375c344dca46b6b0a8fb751d42ca99
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07973047B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート