Hydrochloric Acid → 6-[N-(5-Chloro-2-(2-methylprop-2-en-1-yloxy)benzyl)-N-ethylamino]-3-cyanopyridazine

HRID 1870774

반응식

HRID 1870774 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:21][CH2:22][C:23]([CH3:25])=[CH2:24])=[C:6]([CH:20]=1)[CH2:7][N:8]([C:11]1[N:16]=[N:15][C:14]([C:17]([NH2:19])=O)=[CH:13][CH:12]=1)[CH2:9][CH3:10].CS(Cl)(=O)=O.Cl>N1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:21][CH2:22][C:23]([CH3:25])=[CH2:24])=[C:6]([CH:20]=1)[CH2:7][N:8]([C:11]1[N:16]=[N:15][C:14]([C:17]#[N:19])=[CH:13][CH:12]=1)[CH2:9][CH3:10]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 31297Methanesulfonyl chlorideHCID 186932586-[N-(5-Chloro-2-(2-methylprop-2-en-1-yloxy)benzyl)-N-ethylamino]pyridazine-3-carboxamide

생성물 1

HCID 186932386-[N-(5-Chloro-2-(2-methylprop-2-en-1-yloxy)benzyl)-N-ethylamino]-3-cyanopyridazine수율 126.4%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a solution of 6-[N-(5-chloro-2-(2-methylprop-2-en-1-yloxy)benzyl)-N-ethylamino]-pyridazine-3-carboxamide (example 18) (210 mg, 0.6 mmol) in pyridine (10 ml) at 0° C. was added methane sulfonyl chloride (0.5 ml, 0.6 mmol) and the mixture allowed to stir (gradually coming to an ambient temperature as the ice melts) for 60 hours. The solution was poured into 2 N hydrochloric acid (50 ml) over ice and the product extracted with diethyl ether (200 ml), washed with water (3×200 ml), dried over anhydrous magnesium sulphate and the solvent removed in vacuo to give the title compound as a brown gum (260 mg) which was used without further purification.

후처리

  1. customfor 60 hours
  2. extractionthe product extracted with diethyl ether (200 ml)
  3. washwashed with water (3×200 ml)
  4. dry with materialdried over anhydrous magnesium sulphate
  5. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-28fd233580a849cf9c7979c101dbe3ca
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06100258

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