Benzyl chloroformate → HCID 136338685, 화합물

HRID 967712

반응식

HRID 967712 반응식
[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

참가 물질

7

반응물 3

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

생성물 1

HCID 136338685HCID 136338685, 화합물

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 8028Tetrahydrofuran용매HCID 25517Ammonium Chloride용매

실험 절차

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+).

후처리

  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%)

출처 및 근거

ORD 기록
ord-15eebb5cb7174286965319061605306f
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06956036B1

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