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Benzyl Bromide → 5-Isopropyl-2,4-bis-methoxymethoxy-benzoic acid hydrazide

HRID 1947175
ノート
印刷プレビュー

反応式

HRID 1947175 の反応式
[CH:1]([C:4]1[C:5]([O:17][CH2:18][O:19][CH3:20])=[CH:6][C:7]([O:13][CH2:14][O:15][CH3:16])=[C:8]([CH:12]=1)[C:9](O)=[O:10])([CH3:3])[CH3:2].C(Br)C1C=CC=CC=1.O.[NH2:30][NH2:31]>O1CCCC1>[CH:1]([C:4]1[C:5]([O:17][CH2:18][O:19][CH3:20])=[CH:6][C:7]([O:13][CH2:14][O:15][CH3:16])=[C:8]([CH:12]=1)[C:9]([NH:30][NH2:31])=[O:10])([CH3:3])[CH3:2]
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 7498Benzyl BromideHCID 24654Hydrazine hydrate (1:1)HCID 58236465HCID 58236465、化合物

生成物 1

HCID 598298425-Isopropyl-2,4-bis-methoxymethoxy-benzoic acid hydrazide収率 82%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

5-isopropyl-2,4-bis-methoxymethoxy-benzoic acid (IM3-a: 2.84 g, 10 mmol), N,N′-carbonyldiimidazole (1.62 g, 10 mmol) and tetrahydrofuran 100 mL were placed in a 300 mL eggplant shaped flask and stirred at room temperature for 4 hours. The reaction mixture was mixed with benzylbromide (1.19 mL, 10 mL), stirred at room temperature for further 4 hours and then mixed with hydrazine mono hydrate (0.63 mL, 13 mmol) and stirred at room temperature overnight. After completing the reaction, most of the reaction mixture was removed under reduced pressure, and the residue was mixed with ethyl acetate. The organic layer was washed with saturated sodium hydrogen carbonate and saturated sodium chloride solutions, dried over anhydrous sodium sulfate. After filtration and evaporation, the residue was purified by silica gel column chromatography to obtain the title compound (IM4-a: 2.44 g, 82%).

後処理

  1. stirringstirred at room temperature for further 4 hours
  2. stirringstirred at room temperature overnight
  3. customthe reaction
  4. custommost of the reaction mixture was removed under reduced pressure
  5. additionthe residue was mixed with ethyl acetate
  6. washThe organic layer was washed with saturated sodium hydrogen carbonate and saturated sodium chloride solutions
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationAfter filtration and evaporation
  9. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-9204064c08064226a999c45e2fe07682
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399464B2

反応ノート

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