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Acetic Acid → 6-Isoquinolinecarboxylic acid, methyl ester

HRID 2289495
ノート
印刷プレビュー

反応式

HRID 2289495 の反応式
[CH:1]1[C:10]2[C:5](=[CH:6][C:7]([CH:11]=[O:12])=[CH:8][CH:9]=2)[CH:4]=[CH:3][N:2]=1.[C:13](O)(=[O:15])C>[C-]#N.[Na+].O=[Mn]=O>[CH:1]1[C:10]2[C:5](=[CH:6][C:7]([C:11]([O:15][CH3:13])=[O:12])=[CH:8][CH:9]=2)[CH:4]=[CH:3][N:2]=1
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 176Acetic AcidHCID 15290359Isoquinoline-6-carboxaldehyde

生成物 1

HCID 152903606-Isoquinolinecarboxylic acid, methyl ester

試薬・触媒・溶媒 2

HCID 14801Manganese dioxide触媒HCID 8929Sodium Cyanide溶媒

実験手順

290 mg of isoquinoline-6-carbaldehyde are dissolved in 40 ml of MeON, and firstly 450 mg of NaCN, then 210 μl of glacial acetic acid, and finally 3.5 g of MnO2 are added. The mixture is stirred at RT for 3 days, and the precipitate is filtered off and the filtrate is poured into a solution of 15 g of FeSO4 in 150 ml of water. Subsequently, the pH of the mixture is adjusted to 9 with Na2CO3 solution, the precipitate is filtered off, and the filtrate is extracted 3× with 150 ml of EA. Drying takes place over Na2SO4, and the solvent is removed in vacuo. 190 mg are obtained of a colorless oil, which in reacted without any further purification.

後処理

  1. filtrationthe precipitate is filtered off
  2. additionthe filtrate is poured into a solution of 15 g of FeSO4 in 150 ml of water
  3. filtrationthe precipitate is filtered off
  4. extractionthe filtrate is extracted 3× with 150 ml of EA
  5. customDrying
  6. customthe solvent is removed in vacuo
  7. custom190 mg are obtained of a colorless oil, which
  8. customin reacted without any further purification

出典と根拠

ORDレコード
ord-412978cf007f4a3da45f23db6bad96f1
出典データセット
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06093729

反応ノート

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