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Trifluoroacetic acid → HCID 178434010、化合物

HRID 413300
ノート
印刷プレビュー

反応式

HRID 413300 の反応式
C(OC(=O)[NH:7][CH2:8][CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][C:18]2[NH:22][C:21]([CH3:23])=[N:20][N:19]=2)=[CH:13][CH:12]=1)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[CH3:23][C:21]1[NH:22][C:18]([CH2:17][C:14]2[CH:15]=[CH:16][C:11]([O:10][CH2:9][CH2:8][NH2:7])=[CH:12][CH:13]=2)=[N:19][N:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 178434012HCID 178434012、化合物

生成物 1

HCID 178434010HCID 178434010、化合物収率 45.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of tert-butyl-{2-[4-(5-methyl-4H-[1,2,4]triazol-3-ylmethyl)-phenoxy]-ethyl}-carbamate (380 mg, 1.14 mmol) in methylene chloride (10 ml) was added trifluoroacetic acid (1.7 ml). The resulting mixture was stirred for about thirty minutes and was then concentrated in vacuo. The resulting crude oil was then dissolved in ethyl acetate and brought to pH 10 with aqueous sodium hydroxide. The aqueous layer was extracted with ethyl acetate, and the combined organic extracts were washed with brine, dried over magnesium sulfate, filtered, and concentrated in vacuo to afford 120 mg (45% yield) of the amine product. LRMS ([M+H]+)=233.1.

後処理

  1. concentrationwas then concentrated in vacuo
  2. dissolutionThe resulting crude oil was then dissolved in ethyl acetate
  3. extractionThe aqueous layer was extracted with ethyl acetate
  4. washthe combined organic extracts were washed with brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-5264743f69e34671a0baa65f817b769c
出典データセット
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06566377B2

反応ノート

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