Isopropyl iodide → HCID 178458342, 화합물

HRID 1013839노트

반응식

HRID 1013839 반응식
[Cl:1][C:2]1[CH:23]=[C:22]([OH:24])[CH:21]=[CH:20][C:3]=1[CH2:4][CH:5]1[CH2:9][CH2:8][N:7]([CH:10]2[CH2:18][CH2:17][C:16]3[C:12](=[CH:13][NH:14][N:15]=3)[CH2:11]2)[C:6]1=[O:19].I[CH:26]([CH3:28])[CH3:27].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:23]=[C:22]([O:24][CH:26]([CH3:28])[CH3:27])[CH:21]=[CH:20][C:3]=1[CH2:4][CH:5]1[CH2:9][CH2:8][N:7]([CH:10]2[CH2:18][CH2:17][C:16]3[C:12](=[CH:13][NH:14][N:15]=3)[CH2:11]2)[C:6]1=[O:19]

참가 물질

5

반응물 3

HCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 178515644HCID 178515644, 화합물

생성물 1

HCID 178458342HCID 178458342, 화합물수율 48.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Treat a solution of 3-(2-chloro-4-hydroxy-benzyl)-1-(4,5,6,7-tetrahydro-2H-indazol-5-yl)-pyrrolidin-2-one (0.2 g, 0.58 mmol) and 2-Iodopropane (0.06 mL, 0.64 mmol) in DMF (4 mL) with potassium carbonate (0.1 g, 0.7 mmol) and stir reaction overnight at room temp. Quench the reaction with 1N HCl and extract with EtOAc. Wash the organic with brine, dry over MgSO4, filter, and remove the solvent. Purify the crude by silica gel column chromatography and remove the solvent to afford 0.11 g (48%) of product. MS (m/e): 388 (M+1).

후처리

  1. customreaction overnight at room temp
  2. customQuench
  3. customthe reaction with 1N HCl
  4. extractionextract with EtOAc
  5. washWash the organic with brine
  6. dry with materialdry over MgSO4
  7. filtrationfilter
  8. customremove the solvent
  9. customPurify the crude by silica gel column chromatography
  10. customremove the solvent

출처 및 근거

ORD 기록
ord-e6e220eff38d4711a09fa81e0658c660
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981918B2

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