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Dimethylformamide → 2-benzyl-6-bromo-3-hydroxymethyl-4-phenyl-2H-isoquinolin-1-one

HRID 750132
ノート
印刷プレビュー

反応式

HRID 750132 の反応式
[CH2:1]([N:8]1[C:17]([C:18](O)=[O:19])=[C:16]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([Br:27])[CH:14]=2)[C:9]1=[O:28])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(Cl)(=O)C(Cl)=O.CN(C=O)C>O1CCCC1>[CH2:1]([N:8]1[C:17]([CH2:18][OH:19])=[C:16]([C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([Br:27])[CH:14]=2)[C:9]1=[O:28])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=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 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 230606482-benzyl-6-bromo-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic Acid

生成物 1

HCID 230609532-benzyl-6-bromo-3-hydroxymethyl-4-phenyl-2H-isoquinolin-1-one収率 23%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 2-benzyl-6-bromo-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid (150 mg) in tetrahydrofuran (THF) (5 ml) were added oxalyl chloride (60 μl) and DMF (0.1 ml), and the mixture was stirred at room temperature for 1 hr. The solvent was concentrated under reduced pressure. A solution of the residue in THF (3 ml) was added dropwise to a suspension of sodium borohydride (39 mg) in 1,2-dimethoxyethane. The mixture was stirred under ice-cooling for 1 hr. and poured into 1N hydrochloric acid and the mixture was extracted with ethyl acetate. The extract was washed successively with saturated aqueous sodium hydrogen carbonate and saturated brine, and dried over magnesium sulfate. The solvent was concentrated under reduced pressure and the residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1) to give the title compound (33 mg, 23%).

後処理

  1. concentrationThe solvent was concentrated under reduced pressure
  2. additionA solution of the residue in THF (3 ml) was added dropwise to a suspension of sodium borohydride (39 mg) in 1,2-dimethoxyethane
  3. stirringThe mixture was stirred under ice-
  4. temperaturecooling for 1 hr
  5. additionand poured into 1N hydrochloric acid
  6. extractionthe mixture was extracted with ethyl acetate
  7. washThe extract was washed successively with saturated aqueous sodium hydrogen carbonate and saturated brine
  8. dry with materialdried over magnesium sulfate
  9. concentrationThe solvent was concentrated under reduced pressure
  10. customthe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1)

出典と根拠

ORDレコード
ord-080554b177bb48be819921832bf6890d
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07402595B2

反応ノート

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