O-Phenylenediamine → 1-(4-methoxybenzyl)-2-(4-methoxyphenyl)-1H-benzo(d)imidazole

HRID 338808

反応式

HRID 338808 の反応式
[NH4+].[Br-].[C:3]1([NH2:10])[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH2:9].[CH:11](=O)[C:12]1[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=1>CO>[CH3:19][O:18][C:15]1[CH:16]=[CH:17][C:12]([CH2:11][N:9]2[C:4]3[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=3[N:10]=[C:11]2[C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)=[CH:13][CH:14]=1

参加物

5

反応物 3

HCID 7243O-PhenylenediamineHCID 25514Ammonium BromideHCID 312444-Methoxybenzaldehyde

生成物 1

HCID 7461821-(4-methoxybenzyl)-2-(4-methoxyphenyl)-1H-benzo(d)imidazole収率 38%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In a methanol (5 mL) solvent in the presence of NH4Br (362.3 mg, 3.70 mmol), a solution including 1,2-phenylenediamine (100 mg, 0.92 mmol) and p-anisaldehyde (0.11 mL, 0.82 mmol) was stirred at room temperature for 6 hours, and methanol was evaporated therefrom. The residual was distributed between ethyl acetate and water. An organic layer was dried by using MgSO4, filtered, and evaporated. The residual was purified by silica gel column chromatography using hexane and ethyl acetate (3:1) to obtain a solid Compound 116.

後処理

  1. custommethanol was evaporated
  2. customAn organic layer was dried
  3. filtrationfiltered
  4. customevaporated
  5. customThe residual was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-59ce6cf1b0b44e61891f939e3809619a
出典データセット
uspto-grants-2014_11
特許番号
US08889881B2

関連ノート

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