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Chloroacetaldehyde → 4-(2-{5-[3-(3-Fluoro-phenyl)-2-oxo-imidazolidin-1-yl]-2-methyl-phenylamino}-oxazol-5-yl)-benzonitrile

HRID 244592
ノート
印刷プレビュー

反応式

HRID 244592 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:22])=[C:6]([NH:8][C:9]2[O:10][C:11]([C:14]3[CH:21]=[CH:20][C:17]([C:18]#[N:19])=[CH:16][CH:15]=3)=[CH:12][N:13]=2)[CH:7]=1.Cl[CH2:24][CH:25]=O.[BH3-]C#N.[Na+].C([O-])(O)=O.[Na+].[F:36][C:37]1[CH:42]=[CH:41][CH:40]=[C:39]([N:43]=[C:44]=[O:45])[CH:38]=1.CC(C)([O-])C.[K+]>C(#N)C.C1(C)C=CC=CC=1.O.C(OCC)(=O)C.C(O)(=O)C>[F:36][C:37]1[CH:38]=[C:39]([N:43]2[CH2:25][CH2:24][N:1]([C:2]3[CH:3]=[CH:4][C:5]([CH3:22])=[C:6]([NH:8][C:9]4[O:10][C:11]([C:14]5[CH:21]=[CH:20][C:17]([C:18]#[N:19])=[CH:16][CH:15]=5)=[CH:12][N:13]=4)[CH:7]=3)[C:44]2=[O:45])[CH:40]=[CH:41][CH:42]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

12

反応物 6

HCID 33ChloroacetaldehydeHCID 1230643-Fluorophenyl isocyanateHCID 516892Sodium BicarbonateHCID 5003444Sodium cyanoborohydrideHCID 177573464-[2-(5-Amino-2-methyl-phenylamino)-oxazol-5-yl]-benzonitrileHCID 23665647Potassium tert-butoxide

生成物 1

HCID 11965364
4-(2-{5-[3-(3-Fluoro-phenyl)-2-oxo-imidazolidin-1-yl]-2-methyl-phenylamino}-oxazol-5-yl)-benzonitrile
収率 45%

試薬・触媒・溶媒 5

HCID 176Acetic Acid溶媒HCID 962Water溶媒HCID 1140Toluene溶媒HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 4-[2-(5-Amino-2-methyl-phenylamino)-oxazol-5-yl]-benzonitrile (558 mg, 2 mmol) and chloroacetaldehyde (50 wt. % in water, 628 mg, 4 mmol) in acetonitril (60 mL), was added at RT NaBH3CN (253 mg, 4 mmol) and dropwise acetic acid (0.4 mL). The mixture was stirred at room temperature 1 h. Ethyl acetate (50 mL) and saturated aqueous NaHCO3 (50 mL) were added. The organic layer was washed with brine (20 mL), dried over MgSO4 and concentrated to give a yellow solid. This was dissolved in toluene (40 mL) and treated with 1-Fluoro-3-isocyanato-benzene (274 mg, 2 mmol) at reflux for 2 h. After evaporation of solvent under reduced vacuum, the crude product was dissolved in isopropanol (60 mL) and treated with potassium tert-butoxide (1.8 g, 16 mmol) at RT for 5 h. Water (20 mL) was added, the organic layer was separated dried over MgSO4 and concentrated. The crude product was silica gel column chromatographed (dichloromethane/ethanol: 95/5) to give 408 mg (45%) of the title compound as a beige solid.

後処理

  1. washThe organic layer was washed with brine (20 mL)
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated
  4. customto give a yellow solid
  5. temperatureat reflux for 2 h
  6. customAfter evaporation of solvent under reduced vacuum
  7. dissolutionthe crude product was dissolved in isopropanol (60 mL)
  8. customthe organic layer was separated
  9. dry with materialdried over MgSO4
  10. concentrationconcentrated
  11. customchromatographed (dichloromethane/ethanol: 95/5)

出典と根拠

ORDレコード
ord-edc51a882ed8418e8057a0815757bbe6
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658659B2

反応ノート

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