Isopropyl iodide → HCID 178458342、化合物

HRID 1013839ノート

反応式

HRID 1013839 の反応式
[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]

参加物

5

反応物 3

HCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 178515644HCID 178515644、化合物

生成物 1

HCID 178458342HCID 178458342、化合物収率 48.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e6e220eff38d4711a09fa81e0658c660
出典データセット
uspto-grants-2011_07
特許番号
US07981918B2

反応ノート

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