Benzyl chloroformate → benzyl 2-(6-hydroxy-1H-indazol-1-yl)-1-methylethylcarbamate

HRID 967712

反応式

HRID 967712 の反応式
[NH2:1][CH:2]([CH3:14])[CH2:3][N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([OH:13])[CH:11]=2)[CH:6]=[N:5]1.C(=O)(O)[O-].[Na+].Cl[C:21]([O:23][CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:22]>C1COCC1.Cl.[Cl-].[NH4+]>[CH2:24]([O:23][C:21](=[O:22])[NH:1][CH:2]([CH3:14])[CH2:3][N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([OH:13])[CH:11]=2)[CH:6]=[N:5]1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

参加物

7

反応物 3

HCID 10387Benzyl chloroformateHCID 516892Sodium BicarbonateHCID 1354093531-(2-aminopropyl)-1H-indazol-6-ol

生成物 1

HCID 136338685benzyl 2-(6-hydroxy-1H-indazol-1-yl)-1-methylethylcarbamate

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 8028Tetrahydrofuran溶媒HCID 25517Ammonium Chloride溶媒

実験手順

To a solution of 1-(2-aminopropyl)-indazol-6-ol (0.46 g, 2.4 mmol) in THF (10.0 mL) was added a saturated aqueous solution of sodium bicarbonate (2.0 mL) followed by benzyl chloroformate (0.40 mL) at room temperature. After stirring for 1 h, the solution was diluted with 1 N HCl (10 mL) and ammonium chloride (20 mL) followed by extraction with ethyl acetate (3×50 mL). The combined extracts were washed with brine (10 mL), dried (MgSO4) and evaporated to give a residue which was used in the next step without further purification (0.75 g, 98%); MS (ES) m/z 326 (M+).

後処理

  1. extractionfollowed by extraction with ethyl acetate (3×50 mL)
  2. washThe combined extracts were washed with brine (10 mL)
  3. dry with materialdried (MgSO4)
  4. customevaporated
  5. customto give a residue which
  6. customwas used in the next step without further purification (0.75 g, 98%)

出典と根拠

ORDレコード
ord-15eebb5cb7174286965319061605306f
出典データセット
uspto-grants-2005_10
特許番号
US06956036B1

関連ノート

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