Ethanol → 1-Chloro-4-ethoxyphthalazine

HRID 1852068ノート

反応式

HRID 1852068 の反応式
[Na].Cl[C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]([Cl:13])=[N:5][N:4]=1.[CH3:14][CH2:15][OH:16]>>[Cl:13][C:6]1[C:7]2[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:3]([O:16][CH2:15][CH3:14])=[N:4][N:5]=1

参加物

4

反応物 3

HCID 702EthanolHCID 784901,4-DichlorophthalazineHCID 5360545Sodium

生成物 1

HCID 212176601-Chloro-4-ethoxyphthalazine

実験手順

Sodium (33.8 mg, 1.470 mmol) was allowed to react with EtOH (10 mL), then 1,4-dichlorophthalazine (279 mg, 1.4 mmol) was added and the reaction mixture was refluxing for 30 min. The hot solution was filtered and evaporated. The crude product was purified by silica gel chromatography eluting with 20% ethyl acetate in hexane to give 200 mg of the crude product 1-chloro-4-ethoxyphthalazine. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 8.29-8.18 (m, 2H), 7.99-7.90 (m, 2H), 4.73 (q, J=7.1 Hz, 2H), 1.57 (t, J=7.2 Hz, 3H); MS: MS m/z 209.06 (M++1).

後処理

  1. temperaturethe reaction mixture was refluxing for 30 min
  2. filtrationThe hot solution was filtered
  3. customevaporated
  4. customThe crude product was purified by silica gel chromatography
  5. washeluting with 20% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-ede7a9f42302493888ca5b8b8e5e4b34
出典データセット
uspto-grants-2015_02
特許番号
US08957203B2

反応ノート

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