Tetrahydrofuran → 3-Chloro-6-methoxypyridazine

HRID 454821

반응식

HRID 454821 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 744033-Chloro-6-methoxypyridazine수율 90%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f94eb002897047a8bebf9c0993e81a45
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08497260B2

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