Methyl iodide → HCID 66864160、化合物

HRID 2093095

反応式

HRID 2093095 の反応式
[NH:1]1[C:9]2[CH2:8][CH2:7][N:6]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:5][C:4]=2[CH:3]=[C:2]1[C:17]([O:19][CH2:20][CH3:21])=[O:18].[H-].[Na+].[CH3:24]I>C1COCC1>[CH3:24][N:1]1[C:9]2[CH2:8][CH2:7][N:6]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:5][C:4]=2[CH:3]=[C:2]1[C:17]([O:19][CH2:20][CH3:21])=[O:18]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 668643095-Tert-butyl 2-ethyl 6,7-dihydro-1H-pyrrolo[3,2-C]pyridine-2,5(4H)-dicarboxylate

生成物 1

HCID 66864160HCID 66864160、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 5-tert-butyl 2-ethyl 1,4,6,7-tetrahydro-5H-pyrrolo[3,2-c]pyridine-2,5-dicarboxylate (1.0 eq) in THF at 0° C. was added NaH (1.2 eq) and stirred for half an hour at room temperature. Methyl iodide (1.3 eq) was added and resulting reaction mixture was stirred for 3 hrs. Reaction mixture was then quenched with water and extracted with ethyl acetate, dried over sodium sulphate and concentrated to dryness. Crude mass was then purified by silica gel column chromatography to afford 5-tert-butyl 2-ethyl 1-methyl-1,4,6,7-tetrahydro-5H-pyrrolo[3,2-c]pyridine-2,5-dicarboxylate.

後処理

  1. customresulting
  2. customreaction mixture
  3. stirringwas stirred for 3 hrs
  4. customReaction mixture
  5. customwas then quenched with water
  6. extractionextracted with ethyl acetate
  7. dry with materialdried over sodium sulphate
  8. concentrationconcentrated to dryness
  9. customCrude mass was then purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-bd144e7436764823bf42c0c4d1686669
出典データセット
uspto-grants-2013_05
特許番号
US08440830B2

関連ノート

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