Sodium Hydroxide → 1-(1-(4-fluorophenyl)-1H-indazol-5-yl)-3-methylbutan-1-one

HRID 563412

反応式

HRID 563412 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:16]3[C:11](=[CH:12][C:13]([CH:17]([OH:22])[CH2:18][CH:19]([CH3:21])[CH3:20])=[CH:14][CH:15]=3)[CH:10]=[N:9]2)=[CH:4][CH:3]=1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.[OH-].[Na+]>C(Cl)Cl>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[C:16]3[C:11](=[CH:12][C:13]([C:17](=[O:22])[CH2:18][CH:19]([CH3:20])[CH3:21])=[CH:14][CH:15]=3)[CH:10]=[N:9]2)=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 159087TriacetoxyperiodinaneHCID 670061961-(1-(4-fluorophenyl)-1H-indazol-5-yl)-3-methylbutan-1-ol

生成物 1

HCID 670054831-(1-(4-fluorophenyl)-1H-indazol-5-yl)-3-methylbutan-1-one収率 93.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1-(1-(4-Fluorophenyl)-1H-indazol-5-yl)-3-methylbutan-1-ol (650 mg, 2.17 mmol) was dissolved in 50 mL dry DCM and Dess-Martin periodinane (1.0 g, 2.36 mmol) was added. The reaction mixture was stirred for 12 h. The reaction was poured into 1N NaOH and extracted with DCM×3. The organic layers were dried over MgSO4, filtered, and concentrated to give 600 mg (92% yield) of 1-(1-(4-fluorophenyl)-1H-indazol-5-yl)-3-methylbutan-1-one. MS found: (M+H)+=297.

後処理

  1. extractionextracted with DCM×3
  2. dry with materialThe organic layers were dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-6792eecf91774d4aad37ad114fbcb1c5
出典データセット
uspto-grants-2011_11
特許番号
US08067447B2

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