3-Phenylpropyl isocyanate → N-(3-phenylpropyl)-N'-[(2,2-dimethoxy-2-(4-pyridyl)-1-(4-fluorophenyl)ethyl)] urea

HRID 719756ノート

反応式

HRID 719756 の反応式
[CH3:1][O:2][C:3]([O:19][CH3:20])([C:13]1[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=1)[CH:4]([C:6]1[CH:11]=[CH:10][C:9]([F:12])=[CH:8][CH:7]=1)[NH2:5].[N:21]([CH2:24][CH2:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)=[C:22]=[O:23]>C1COCC1>[C:27]1([CH2:26][CH2:25][CH2:24][NH:21][C:22]([NH:5][CH:4]([C:6]2[CH:7]=[CH:8][C:9]([F:12])=[CH:10][CH:11]=2)[C:3]([O:2][CH3:1])([O:19][CH3:20])[C:13]2[CH:18]=[CH:17][N:16]=[CH:15][CH:14]=2)=[O:23])[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1

参加物

4

反応物 2

HCID 34276663-Phenylpropyl isocyanateHCID 219018732,2-Dimethoxy-2-(4-pyridyl)-1-(4-fluorophenyl)ethanamine

生成物 1

HCID 21901874N-(3-phenylpropyl)-N'-[(2,2-dimethoxy-2-(4-pyridyl)-1-(4-fluorophenyl)ethyl)] urea

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 2,2-dimethoxy-2-(4-pyridyl)-1-(4-fluorophenyl)ethanamine (1.22 g, 4.4 mmol) in THF (10 mL) was added a solution of (3-isocyanatopropyl)-benzene (1.61 g, 10 mmol) in THF (10 mL). The resulting mixture was stirred at room temperature for 30 minutes. The reaction was quenched by addition of water (50 mL) and extracted with ethyl acetate (2×50 mL). The combined ethyl acetate extract was washed with water (50 mL), brine (50 mL) and dried with Na2SO4. After removal of solvent, the crude product was purified by column chromatography to yield the product as a light brown solid.

後処理

  1. customThe reaction was quenched by addition of water (50 mL)
  2. extractionextracted with ethyl acetate (2×50 mL)
  3. extractionThe combined ethyl acetate extract
  4. washwas washed with water (50 mL), brine (50 mL)
  5. dry with materialdried with Na2SO4
  6. customAfter removal of solvent
  7. customthe crude product was purified by column chromatography

出典と根拠

ORDレコード
ord-7af0c282d60b4223892d0a22325ba8af
出典データセット
uspto-grants-2006_11
特許番号
US07132544B2

反応ノート

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