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Ethyl Acetate → HCID 59370741、化合物

HRID 1873973
ノート
印刷プレビュー

反応式

HRID 1873973 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([O:11][Si](CC)(CC)CC)[CH2:9]I)=[CH:4][C:3]=1[NH:19][S:20]([CH3:23])(=[O:22])=[O:21].CCCC[N+](CCCC)(CCCC)CCCC.[F-].C1COCC1.C(OCC)(=O)C>C1COCC1.[Cl-].[Na+].O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[CH2:9][O:11]2)=[CH:4][C:3]=1[NH:19][S:20]([CH3:23])(=[O:22])=[O:21]
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 3

HCID 8857Ethyl AcetateHCID 11078149TBAF tetrahydrofuranHCID 53922285HCID 53922285、化合物

生成物 1

HCID 59370741HCID 59370741、化合物収率 50%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

(R)—N-(2-Chloro-5-(2-iodo-1-(triethylsilyloxy)ethyl)phenyl)methanesulfonamide (2.2308 g) was dissolved in dehydrated THF (40 mL), and added with 1 mol/L-TBAF-THF solution (10 mL; manufactured by Sigma-Aldrich Co.), followed by replacement with nitrogen and stirring at room temperature for 1 hour. The reaction solution was added to brine, and extraction was carried out once with ethyl acetate. The organic layer was washed once with water and dried over magnesium sulfate. After the solvent was evaporated under reduced pressure, the resulting residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=71:29→50:50) to obtain the title compound (0.564 g).

後処理

  1. washThe organic layer was washed once with water
  2. dry with materialdried over magnesium sulfate
  3. customAfter the solvent was evaporated under reduced pressure
  4. customthe resulting residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=71:29→50:50)

出典と根拠

ORDレコード
ord-1efa9d0800c64757a83c6b6509cb88ce
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08304443B2

反応ノート

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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