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Triacetoxyperiodinane → tert-butyl 1-(2-(4-chlorophenyl)-4,4,4-trifluoro-1-oxobutan-2-yl)-1H-indazol-4-ylcarbamate

HRID 1427280
ノート
印刷プレビュー

反応式

HRID 1427280 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([N:16]2[C:24]3[C:19](=[C:20]([NH:25][C:26](=[O:32])[O:27][C:28]([CH3:31])([CH3:30])[CH3:29])[CH:21]=[CH:22][CH:23]=3)[CH:18]=[N:17]2)([CH2:11][C:12]([F:15])([F:14])[F:13])[CH2:9][OH:10])=[CH:4][CH:3]=1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>C(Cl)Cl.O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([N:16]2[C:24]3[C:19](=[C:20]([NH:25][C:26](=[O:32])[O:27][C:28]([CH3:30])([CH3:29])[CH3:31])[CH:21]=[CH:22][CH:23]=3)[CH:18]=[N:17]2)([CH2:11][C:12]([F:14])([F:15])[F:13])[CH:9]=[O:10])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 70561960tert-butyl 1-(2-(4-chlorophenyl)-4,4,4-trifluoro-1-hydroxybutan-2-yl)-1H-indazol-4-ylcarbamate

生成物 1

HCID 86705054tert-butyl 1-(2-(4-chlorophenyl)-4,4,4-trifluoro-1-oxobutan-2-yl)-1H-indazol-4-ylcarbamate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of the product of Step B (200 mg, 0.42 mmol) in DCM (5 mL) was added Dess-Martin periodinane (350 mg, 0.84 mmol) in portion at room temperature. The mixture was stirred at for 0.5 h, and then diluted with water (5 mL), extracted with ethyl acetate. The organic layers were washed with brine (5 mL), dried over sodium sulfate, filtered and evaporated. The residue was purified by silica gel chromatography (EA/PE=1:8) to afford the title compound. LC/MS m/z=468.2[M+H]+.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layers were washed with brine (5 mL)
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was purified by silica gel chromatography (EA/PE=1:8)

出典と根拠

ORDレコード
ord-ba5708bb8f6e4e02b673d8fdc89de931
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08933113B2

反応ノート

読み込み中…

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