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Sodium Thiosulfate → 3-cyano-N-[2-(4-cyanophenyl)-4-oxobutyl]-N-methyl-1-naphthamide

HRID 749449
ノート
印刷プレビュー

反応式

HRID 749449 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([C:13]([N:15]([CH2:17][CH:18]([C:22]2[CH:27]=[CH:26][C:25]([C:28]#[N:29])=[CH:24][CH:23]=2)[CH2:19][CH2:20][OH:21])[CH3:16])=[O:14])[C:6]2[C:11]([CH:12]=1)=[CH:10][CH:9]=[CH:8][CH:7]=2)#[N:2].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.S([O-])([O-])(=O)=S.[Na+].[Na+]>C(Cl)Cl.C([O-])(O)=O.[Na+]>[C:1]([C:3]1[CH:4]=[C:5]([C:13]([N:15]([CH2:17][CH:18]([C:22]2[CH:23]=[CH:24][C:25]([C:28]#[N:29])=[CH:26][CH:27]=2)[CH2:19][CH:20]=[O:21])[CH3:16])=[O:14])[C:6]2[C:11]([CH:12]=1)=[CH:10][CH:9]=[CH:8][CH:7]=2)#[N: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 24477Sodium ThiosulfateHCID 159087TriacetoxyperiodinaneHCID 689764513-cyano-N-[2-(4-cyanophenyl)-4-hydroxybutyl]-N-methyl-1-naphthamide

生成物 1

HCID 112690383-cyano-N-[2-(4-cyanophenyl)-4-oxobutyl]-N-methyl-1-naphthamide収率 43%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒
HCID 516892
Sodium Bicarbonate
溶媒

実験手順

3-Cyano-N-[2-(4-cyanophenyl)-4-hydroxybutyl]-N-methyl-1-naphthamide (0.70 g, 1.8 mmol) was dissolved in CH2Cl2 (15 mL) and to the resultant solution was added Dess Martin Periodinane (0.85 g, 2.0 mmol) in portions. The mixture was stirred at room temperature overnight and then sodium thiosulfate (1.9 g, 12 mmol), dissolved in saturated NaHCO3 solution (30 mL), was added. The mixture was stirred vigorously for 2 h and then the organic solution was washed with brine and dried over Na2SO4. The solvent was removed by evaporation and the residue purified by flash chromatography (ethyl acetate-heptane, 4:1). There was obtained 0.50 g, (43%) of 3-cyano-N-[2-(4-cyanophenyl)-4-oxobutyl]-N-methyl-1-naphthamide as a white solid. 1H NMR (400 MHz, CDCl3): 2.7 (s, 3H), 2.9-4.4 (cm, 5H), 6.4-7.8 (cm, 8H), 7.9 (d, 1H), 8.2 (s, 1H), 9.8 (s, 1H); LCMS: m/z 382 (M+1)+.

後処理

  1. additionwas added
  2. stirringThe mixture was stirred vigorously for 2 h
  3. washthe organic solution was washed with brine
  4. dry with materialdried over Na2SO4
  5. customThe solvent was removed by evaporation
  6. customthe residue purified by flash chromatography (ethyl acetate-heptane, 4:1)

出典と根拠

ORDレコード
ord-cd710ff6b9994fe7abe809df7a783698
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07402581B2

反応ノート

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