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HCID 14993733、化合物 → 5,6-Dimethoxy-2-methylisoindoline

HRID 1032488
ノート
印刷プレビュー

反応式

HRID 1032488 の反応式
[I-].[CH2:2]([N+:9]1(C)[CH2:17][C:16]2[C:11](=[CH:12][C:13]([O:20][CH3:21])=[C:14]([O:18][CH3:19])[CH:15]=2)[CH2:10]1)C1C=CC=CC=1.[H][H]>CO.[C].[Pd]>[CH3:19][O:18][C:14]1[CH:15]=[C:16]2[C:11](=[CH:12][C:13]=1[O:20][CH3:21])[CH2:10][N:9]([CH3:2])[CH2:17]2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14993733HCID 14993733、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 190214005,6-Dimethoxy-2-methylisoindoline

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

1.0 g (2.43 mmol) of N-benzyl-5,6-dimethoxy-N-methylisoindolinium iodide was dissolved in 40 ml of a 50% methanol aqueous solution, and 300 mg of a 10% palladium carbon catalyst was added. Then, the catalytic reduction was conducted at 50° C. for 6 hours in a hydrogen gas stream. After filtering off the catalyst, methanol was distilled off under reduced pressure, and the residual solution was adjusted to strongly alkaline by an addition of a 50% sodium hydroxide aqueous solution. Then, the solution was extracted twice with methylene chloride. The extract solution was dried over anhydrous sodium sulfate, and the solvent was distilled off to obtain 200 mg of the above identified compound.

後処理

  1. additionwas added
  2. filtrationAfter filtering off the catalyst, methanol
  3. distillationwas distilled off under reduced pressure
  4. additionto strongly alkaline by an addition of a 50% sodium hydroxide aqueous solution
  5. extractionThen, the solution was extracted twice with methylene chloride
  6. dry with materialThe extract solution was dried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled off
  8. customto obtain 200 mg of the

出典と根拠

ORDレコード
ord-93663239eea44b2b850f0c9f0d312007
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04958029

反応ノート

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