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

HRID 1427228ノート

反応式

HRID 1427228 の反応式
CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.[Cl:23][C:24]1[CH:29]=[CH:28][C:27]([C:30]([N:35]2[C:43]3[C:38](=[C:39]([NH:44][C:45](=[O:51])[O:46][C:47]([CH3:50])([CH3:49])[CH3:48])[CH:40]=[CH:41][CH:42]=3)[CH:37]=[N:36]2)([CH2:33][CH3:34])[CH2:31][OH:32])=[CH:26][CH:25]=1>C(Cl)Cl>[Cl:23][C:24]1[CH:29]=[CH:28][C:27]([C:30]([N:35]2[C:43]3[C:38](=[C:39]([NH:44][C:45](=[O:51])[O:46][C:47]([CH3:50])([CH3:49])[CH3:48])[CH:40]=[CH:41][CH:42]=3)[CH:37]=[N:36]2)([CH2:33][CH3:34])[CH:31]=[O:32])=[CH:26][CH:25]=1

参加物

4

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 70560487tert-butyl 1-(2-(4-chlorophenyl)-1-hydroxybutan-2-yl)-1H-indazol-4-ylcarbamate

生成物 1

HCID 86705040tert-butyl 1-[2-(4-chlorophenyl)-1-oxobutan-2-yl]-1H-indazol-4-ylcarbamate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of Dess-Martin periodinane (8.12 g, 19.15 mmol) in DCM (90 mL) at 0° C. was added a solution of tert-butyl 1-[2-(4-chlorophenyl)-1-hydroxybutan-2-yl]-1H-indazol-4-ylcarbamate (3.18 g, 7.67 mmol) in DCM (20 mL). The mixture was allowed to stir at rt for 2 hours. Then it was filtered and the filtrate was concentrated in vacuo to afford the crude product. The product was purified via column chromatography (0-10% EtOAc/hexanes) to provide the desired product.

後処理

  1. filtrationThen it was filtered
  2. concentrationthe filtrate was concentrated in vacuo
  3. customto afford the crude product
  4. customThe product was purified via column chromatography (0-10% EtOAc/hexanes)

出典と根拠

ORDレコード
ord-d5462192b8f1474b8b971b6715017dfd
出典データセット
uspto-grants-2015_01
特許番号
US08933113B2

反応ノート

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