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Methanol → 5,6-Dihydroxy-N-methylisoindoline hydrobromide

HRID 1032489
ノート
印刷プレビュー

反応式

HRID 1032489 の反応式
[Br-:1].[CH2:2]([N+:9]1(C)[CH2:17][C:16]2[C:11](=[CH:12][C:13]([OH:19])=[C:14]([OH:18])[CH:15]=2)[CH2:10]1)C1C=CC=CC=1.CO.[H][H]>[C].[Pd].C(O)(=O)C>[BrH:1].[OH:19][C:13]1[CH:12]=[C:11]2[C:16](=[CH:15][C:14]=1[OH:18])[CH2:17][N:9]([CH3:2])[CH2:10]2
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 887MethanolHCID 14993734N-benzyl-5,6-dihydroxy-N-methylisoindolinium bromideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 140984225,6-Dihydroxy-N-methylisoindoline hydrobromide

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 176Acetic Acid溶媒

実験手順

1.0 g (2.97 mmol) of N-benzyl-5,6-dihydroxy-N-methylisoindolinium bromide obtained in Example 4 was dissolved in a solution comprising 10 ml of methanol and 10 ml of acetic acid, and 300 mg of a 10% palladium carbon catalyst was added thereto. Then, the catalytic reduction was conducted at 60° C. for 6 hours in a hydrogen gas stream. After filtering off the catalyst, the filtrate was evaporated to dryness under reduced pressure. To the residue, 10 ml of methanol was added, and the mixture was left to cool. The precipitated crystals were collected by filtration and washed with 10 ml of acetone to obtain 500 mg of the above identified compound as white crystals.

後処理

  1. additionwas added
  2. filtrationAfter filtering off the catalyst
  3. customthe filtrate was evaporated to dryness under reduced pressure
  4. additionTo the residue, 10 ml of methanol was added
  5. waitthe mixture was left
  6. temperatureto cool
  7. filtrationThe precipitated crystals were collected by filtration
  8. washwashed with 10 ml of acetone
  9. customto obtain 500 mg of the

出典と根拠

ORDレコード
ord-1d3cb6fe86164c3e927cd40d5058adb7
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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