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Water → HCID 12777809、化合物

HRID 2390023
ノート
印刷プレビュー

反応式

HRID 2390023 の反応式
CON(C)[C:4]([CH2:6][C:7]1[N:8]=[CH:9][C:10]2[C:15]([CH:16]=1)=[CH:14][CH:13]=[CH:12][CH:11]=2)=O.[C:18]1([Mg]Br)C=[CH:22][CH:21]=[CH:20][CH:19]=1.[OH2:26]>C1COCC1>[C:6]([C:7]1[N:8]=[CH:9][C:10]2[C:15]([CH:16]=1)=[CH:14][CH:13]=[CH:12][CH:11]=2)(=[O:26])[C:4]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=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 3

HCID 962WaterHCID 131729961HCID 131729961、化合物HCID 178418255HCID 178418255、化合物

生成物 1

HCID 12777809HCID 12777809、化合物収率 77%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Under an argon gas stream, 168 mg of N-methoxy-N-methylisoquinoline-3-carboxyamide was dissolved in 1 mL of anhydrous THF, followed by stirring under cooling with ice. To the reaction liquid was slowly added 0.8 mL of phenyl magnesium bromide (1 mol/L THF solution), followed by continuously stirring for 30 minutes. Water was added to the reaction liquid, followed by extraction with chloroform. The organic layer was washed with diluted hydrochloric acid and saturated brine, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The residue obtained was purified by silica gel chromatography (chloroform alone) to obtain 154 mg (yield 77%) of a title compound as a yellow oily substance.

後処理

  1. temperatureunder cooling with ice
  2. customTo the reaction liquid
  3. stirringby continuously stirring for 30 minutes
  4. extractionfollowed by extraction with chloroform
  5. washThe organic layer was washed with diluted hydrochloric acid and saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue obtained
  9. customwas purified by silica gel chromatography (chloroform alone)

出典と根拠

ORDレコード
ord-ac6f507ba7934ea3a6b7c75b7ecf6167
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08273766B2

反応ノート

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