Tetrahydrofuran → 3-Chloro-6-methoxypyridazine

HRID 454821

反応式

HRID 454821 の反応式
CO.C[O-].[Na+].[O:6]1CCC[CH2:7]1.[Cl:11][C:12]1[N:13]=[N:14][C:15](Cl)=[CH:16][CH:17]=1>O>[CH3:7][O:6][C:15]1[N:14]=[N:13][C:12]([Cl:11])=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 673313,6-DichloropyridazineHCID 23694274Sodium methanolate methanol

生成物 1

HCID 744033-Chloro-6-methoxypyridazine収率 90%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A 0.5 M sodium methoxide methanol solution (NaOMe in MeOH, 7.4 mL, 3.69 mmol) was slowly added to an anhydrous tetrahydrofuran (12 mL) solution having 3,6-dichloropyridazine (107, 500 mg, 3.36 mmol) dissolved therein, stirred at room temperature for one hour, followed by adding water. Organic compounds were extracted with ethyl acetate. Then, the recovered organic solution was washed with an aqueous solution of saturated sodium chloride and evaporated after a treatment with sodium sulfate. Purification was performed by column chromatograph to give the target compound 3-methoxy-6-chloropyridazine (108a, 436 mg, 90%) as a white solid.

後処理

  1. dissolutiondissolved
  2. extractionOrganic compounds were extracted with ethyl acetate
  3. washThen, the recovered organic solution was washed with an aqueous solution of saturated sodium chloride
  4. customevaporated after a treatment with sodium sulfate
  5. customPurification

出典と根拠

ORDレコード
ord-f94eb002897047a8bebf9c0993e81a45
出典データセット
uspto-grants-2013_07
特許番号
US08497260B2

関連ノート

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